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May 2019
Preservatives and
Thickeners vs.
Active Release
Dry Masks
for Direct
Delivery
Collagen
Fragmentation
Jasmine Rice
Whitening
and Skin Protection
WANT MORE?
Check out our digital edition exclusives!
www.CosmeticsandToiletries.com/DE
CT1905_Cover_fcx.indd 1 4/16/19 3:58 PM

Cover Story Contents | C&T
May 2019 | Volume 134, number 5
6 Editor’s Note
®
Anti-aging About-face
10 Industry Insight
Flexing Beauty Biceps: How Muscle
Controls Hyperpigmentation
10 [video] How Muscle Controls

DIGITAL
EDITION Facial Hyperpigmentation
with S. Nishikori
Visit cosmeticsandtoiletries.com/DE
26
for your Digital Edition.
72 Ad Index
Research
26 Youth in Yields
Jasmine Rice Extract Whitens, Protects
and Smooths Skin
by M. Kanlayavattanakul, N. Lourith, Ph.D., and P. Chaikul
DE3 Microbiome Disconnect

DIGITAL
Antibiotics and Dysbiosis: A Commentary
EDITION
by B. Teoh
DE4 [video] A Probiotic-like Approach
34
to Skin Care
DIGITAL
EDITION
A ‘Natural’ Progression
with S. Majeed and A. Sivakumar, Ph.D.
Testing
48 34 Testing Tactics in Skin: Total Breakdown

Recovering Anti-aging Efficacy After
Collagen Fragmentation
by R. Holtz
37 [video] Hyaluronan Homeostasis for

DIGITAL
EDITION Anti-aging Effects
with H. Yoshida
2 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019
CT1905_TOC_Masthead_fcx.indd 2 4/16/19 3:55 PM

FIRST
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Editor’s note | C&T ®
Contents | C&T ®
Formulating
EDITORIAL
42 Ingredient Profile: Vitamin E Editor in Chief Jeb Gleason-Allured | 1-630-344-6069/jallured@allured.com
Defeating Free Radicals Senior Managing Editor Katie Anderson | 1-630-344-6077/kanderson@allured.com
Managing Editor Rachel L. Grabenhofer | 1-630-344-6072/rgrabenhofer@allured.com
by P. Bahadur and S. Narasimhan, Ph.D.
Assistant Editor Brooke Schleehauf | 1-630-344-6032/bschleehauf@allured.com
News Editor Eden Stuart | 630-344-6053/estuart@allured.com
48 Direct Connect
Dry Mask Vectors Drive Active Delivery
ADVERTISING SALES
by B. Mosna, et al.
Business Development Manager Jolly Patel | 1-630-344-6061/jpatel@allured.com
Fragrance Sales Paige Crist | 1-630-344-6060/pcrist@allured.com
58 Active Transport Advertising Coordinator Kasia Smialkowski | 1-630-344-6025/ksmialkowski@allured.com
How Rheology Modifiers and Preservatives
Impact Release AUDIENCE DEVELOPMENT
by R. Polowyj, M. Stevic and S. Tamburic, Ph.D. Marketing Specialist Katy Chitwood
Customer Service 1-847-559-7558/customerservice@cosmeticsandtoiletries.com
58 70 Anti-Aging Formulary
DESIGN
Design Manager
Graphic Designer
Production Manager
CORPORATE
Kim Fry
James Fergus
Bryan Crowe
Partner & CEO George Fox

DE1 Expanded Anti-Aging Formulary Partner & President Janet Ludwig
DIGITAL
EDITION Visit cosmeticsandtoiletries.com/DE CFO Rich Winters
for your Digital Edition. Director of Events Maria Prior
Digital Products Director Rose Southard
Market Intelligence
Executive Assistant Maria Romero
OTHER ALLURED PRODUCTS

12 Technology Launches Cosmetics & Toiletries Bench Reference
Cosmetics & Toiletries magazine: Portuguese edition
Global Cosmetic Industry magazine
15 Product Roundup Beauty Accelerate
Antioxidant and Probiotic Solutions Perfumer & Flavorist magazine
Flavorcon
World Perfumery Congress
16 Consumer Perspective: Skin Inc. magazine
Face & Body Midwest spa expo and conference
Picking Up the Slack Face & Body Northern California spa expo and conference
Sagging Skin as an Anti-aging Target Face & Body Southeast spa expo and conference
by K. Steventon, Ph.D.
For Subscriptions: Subscribe online: www.CosmeticsandToiletries.com/subscribe
For both the US and internationally, telephone: 1-847-559-7558
16 From the Vault: Facial Fat (8 AM–4:30 PM Central, Monday–Friday) Fax: 1-847-291-4816
E-mail: customerservice@cosmeticsandtoiletries.com
DIGITAL
EDITION as a Key Anti-aging Target Address: Cosmetics & Toiletries, PO Box 3009, Northbrook, IL 60065-3009
Print subscriptions: Available free to qualified individuals located in the United States.
Visit cosmeticsandtoiletries.com/DE All other countries may subscribe to the digital edition.
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Cosmetics & Toiletries® (ISSN 0361-4387CTOIDG) is published ten times per year as Jan., Feb., March, April, May, June,
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20 Back to Basics, Part II Address: Cosmetics & Toiletries, 336 Gundersen Drive, Suite A, Carol Stream, IL 60188-2403.
www.CosmeticsandToiletries.com
Ensuring Product Safety All correspondence regarding business, editorial, advertising and production should be sent to Cosmetic & Toiletries,
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additional mailing offices.
POSTMASTER: Send address changes to Cosmetics & Toiletries, PO Box 3009, Northbrook, IL 60065-3009
Allured Business Media makes all attempts to publish accurate information; however, this publication may contain technical
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LinkedIn Facebook inaccuracies, errors or omissions in this publication and in other documentation referred to within or affiliated with
Cosmetics & Toiletries Cosmetics & Toiletries this publication.
Copyright 2019: Reproduction in whole or in part without permission is strictly prohibited.

4 | www.CosmeticsandToiletries.com Vol. 133, No. 10 | November/December 2018
Cosmetics & Toiletries and C&T are registered trademarks of Allured Publishing Corporation.
CT1905_TOC_Masthead_fcx.indd 4 4/16/19 3:55 PM

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Editor’s Note | C&T ®
Anti-aging About-face
The anti-aging category has made an about-face. Consumers are embracing age, recasting
it as wellness or well aging. In fact, skin care itself has emerged as a direct path to preventing
age-related ailments such as Alzheimer’s, heart disease and diabetes; University of California,
San Francisco, dermatologists found that well-moisturized skin produced lower cytokine
levels in blood and, in turn, reduced disease-causing inflammatory signals in the body.1
Anti-aging, however it’s defined, is still a major market driver. Transparency Market
Research2 reported the global skin care market stood at $127.1 billion in 2015 and may
surpass $200 billion by 2024 (a respectable CAGR of 5.1%)—with anti-aging creams leading
the charge, especially for wrinkle minimization. Perhaps the most original and still-trendy
anti-aging ingredients are antioxidants. Many of these are also naturally derived, so they
impact the market from two major angles; the same group projects3 that antioxidants,
including for foods, will reach $3.1 billion by 2020 with similar CAGR of 5.6% (from 2014).
There’s also the matter of delivering products efficiently to their site of action, which is
where technologies like the ever-popular sheet mask come in. The same firm places4 sheet
masks ahead of other categories, with a whopping 8.7% CAGR (2018-2026).
This issue combines these and other closely connected concepts to help you
reshape the anti-aging product category. From vitamin E fundamentals and
a socially responsible Jasmine rice active, to dry sheet mask formulating,
and research in sagging skin, active release and collagen fragmentation, we
hope this anti-aging issue takes your product development efforts in exciting
new directions.
References
1. www.cosmeticsandtoiletries.com/research/universitydata/Skin-Care-Could-
Translate-to-Brain-Heart-and-Blood-Sugar-Health-507298861.html
2. www.transparencymarketresearch.com/pressrelease/cosmetic-skin-care-market.htm Rachel L. Grabenhofer
3. www.transparencymarketresearch.com/pressrelease/antioxidants-market.htm C&T Managing Editor
4. www.transparencymarketresearch.com/sheet-face-masks-market.html
CT1905_Editors_Note_fcx.indd 6 4/23/19 11:05 AM

Scientific Industry Insight | C&T ®
Advisory Board
Flexing Beauty Biceps: How Muscle

Eric Abrutyn
TPC2 Advisors Ltd. Controls Hyperpigmentation
Jean-Christophe Choulot
Caudalíe Working out makes a world of difference for your physical
Zoe Diana Draelos, M.D. and mental well-being, but new research suggests it also
Dermatology impacts beauty in a previously unknown way. According
Consulting Services
to POLA scientists, there is a connection between higher
Angela R. Eppler, Ph.D. muscle mass and the formation of fewer hyperpigmented
Pfizer Consumer Healthcare spots, also known as lentigines.
Shu Nishikori (SN) explained this finding in a recent
Trefor Evans, Ph.D.
TA Evans LLC interview, recorded at the IFSCC Congress in Munich; the
following is an adaptation. To watch the video, visit
S. Peter Foltis www.CosmeticsandToiletries.com/multimedia or click on
L’Oréal
the video below (see Page 10 in your digital edition).
Mindy Goldstein, Ph.D.
Atlantic Coast Media Group
Cosmetics & Toiletries (C&T) : Describe the focus
John Jiménez of your latest study.
SN: My research was about muscles of the body. We found a

Belcorp Colombia
Karl Laden, Ph.D. relationship between muscle mass and skin statuses such as
Alpa Cosmetics lentigines and wrinkles. We observed that people with a higher
muscle mass had a lower number of lentigines, which was
Prithwiraj Maitra, Ph.D.
Johnson & Johnson very interesting, so we attempted to quantify this effect and
the mechanisms of how muscle mass might affect the appear-
Jennifer Marsh, Ph.D. ance of lentigines.
Procter & Gamble
Marc Pissavini, Ph.D. C&T : What did you discover?

SN: We found that myoglycogen,
Coty-Lancaster
Luigi Rigano, Ph.D. which is secreted from muscle,

Industrial Consulting Research
suppresses lentigines. Myoglyco-
Sylvianne Schnebert, M.D. gen is released through our whole
LVMH Recherche body and delivered to the facial
Ron Sharpe
skin, where it affects melanocytes
in the epidermis by suppress-
VIDEO
Amway
ing melanogenesis. Through
Leslie C. Smith, Ph.D. this mechanism, myoglycogen
How Muscle Controls Facial
Hyperpigmentation
Consultant suppresses the appearance
of lentigines.
David C. Steinberg
C&T : What are the next steps
Steinberg & Associates
Peter Tsolis to apply this research?
SN: I think the next step is

The Estée Lauder Companies
Russel Walters, Ph.D. product development, such as

Johnson & Johnson
developing cosmetic items to
Claudie Willemin improve skin status by control-
L’Oréal ling the function of myokines
such as myoglycogen in the skin
Shuliang Zhang, Ph.D. or in the whole body. We could
Coty, Inc.
potentially develop products to
affect the muscle cells and pro-
mote the release of myokines (to
control pigmentation).
CT1905_Industry_Insight_fcx_DE.indd 10 4/23/19 11:14 AM

CREATING TOMORROW’S SOLUTIONS
BEAUTY MEETS
SUSTAINABILITY
BELSIL ® ECO
Sustainable production of beauty products now has a name: BELSIL® eco. WACKER is the first manufacturer in
the world to offer valuable silicones manufactured according to methods that have been certified to conserve
resources – and that use biomethanol from natural sources. This not only conserves fossil-based raw materials:
the use of renewable biobased materials also sets a benchmark when it comes to sustainable production using
silicone ingredients. And you benefit from environmentally friendly silicone additives of consistently high quality.
So use BELSIL® eco and make your production processes responsible and environmentally sound.
More information is available at: www.wacker.com/belsileco www.wacker.com/socialmedia

Technology Launches
Highlighting the latest in cosmetic technology and ingredients;
this month covers delivery enhancers, mood-boosting actives and more.
Skin Care Solvers
Amberstem IBR-UrBioTect
Sederma IFF-Lucas Meyer
www.sederma.com www.lucasmeyercosmetics.com
Sederma launched Amberstem (INCI: Glycerin (and) Barrier function may be improved via IFF-Lucas Meyer’s IBR-UrBioTect
Buddleja Davidii Leaf Cell Extract (and) Xanthan Gum), a (INCU: Inula Helenium Extract), which also reduces blue-light induced
brightener created specifically for olive skin types prone oxidative stress and inflammation to improve skin hydration, radiance
to dullness, dehydration, hypersensitivity and uneven and elasticity. Furthermore, the ingredient prevents the appearance of
complexion. It works by protecting the skin barrier, premature aging due to environmental stressors.
controlling pigmentation and providing anti-inflammation
and antioxidative effects synergistically.
Algaenia
Laboratories Expanscience
www.expanscience.com
Based on microalgae, Algaenia (INCI: Glyc-
erin (and) Propanediol (and) Water (aqua)
(and) Chlamydomonas Acidophila Extract)
is meant to protect sensitive and reactive
skin by moderating inflammation and red-
ness while moisturizing and soothing.
Sensityl
Givaudan Active Beauty
Hair Conditioner www.givaudan.com
Givaudan Active Beauty’s Sensityl (INCI:
AminoSensyl HC Not Available) is an indirect mood-
INOLEX influencer meant to provide soothing
www.inolex.com benefits that, in turn, help consumers to
INOLEX unveiled AminoSensyl HC (INCI: Brassica think positively about their skin. The active
Alcohol (and) Brassicyl Valinate Esylate), a pre- works epigenetically and is recommended
neutralized natural hair care active system that for use in sensitive skin applications,
offers performance and ease of formulation for shampoo, aftershave and more.
hair conditioning and treatment products. The
active also delivers strengthening, conditioning,
smoothness and definition in hair applications.
CT1905_Tech_Launches_fcx.indd 12 4/16/19 4:25 PM

Makeup
SpectraFlex Illusion Pigments

Sun Chemical
www.sunchemical.com
SpectraFlex Illusion Pigments (INCI:
Not Available) were developed to
balance transparency and diffuse
transmission and reflectivity. They
can be used in soft-focus color, Cosmospheres
skin care and body care formula- Omya
tions, including in makeup primers. www.omya.com
Omya has launched Cosmospheres (INCI: Varies), brightly
colored beads that can be loaded with actives to enhance
delivery and aesthetic optical effects. The beads can also dis-
pense pigments, or be used as cooling and warming agents,
fragrances, functional ingredients and other substances.
Natural and Sustainable

JD Jojoba Butter Vegan
Jojoba Desert
www.jojobadesert.com
JD Jojoba Butter Vegan (INCI: Not
Available) leaves behind the same
soft, silky feeling as its original JD
Jojoba Butter counterpart but con-
tains a high concentration of jojoba
oil, is oil-miscible and is free of
preservatives and coloring agents.
InstaMask Shale with

Vitamin C & Aloe Vera
Vantage
Avenaplex www.vantagegrp.com
Oat Cosmetics Enabling the personalization trend and
www.oatcosmetics.com waterless formulating, Vantage’s bead-like
Avenaplex (INCI: Avena Sativa (Oat) InstaMask Shale with Vitamin C & Aloe Vera
Kernel Extract) is a natural complex of (INCI: Kaolin (and) Aluminum Silicate (and)
skin-identical lipids meant to protect Mannitol (and) Cellulose (and) PVP (and)
aged skin by repairing the skin barrier, Sodium Polyacrylate (and) Hydroxypropyl
replenishing skin lipids and increasing Methylcellulose (and) Aloe Barbadensis
ceramide levels. Leaf Juice (and) Ascorbic Acid) contains the
clays, actives and thickeners needed for a
mask so that consumers can add a second-
ary booster for a DIY, mess-free and gently
exfoliating product.
Vol. 134, No. 5 | May 2019 Cosmetics & Toiletries® | 13
CT1905_Tech_Launches_fcx.indd 13 4/18/19 11:33 AM

Technology Launches
Anti-aging Innovations
cb2-skin Nephoria
Ashland BASF
www.ashland.com www.carecreations.basf.com
Patchouli-based cb2-skin (INCI: Pogostemon Cablin Leaf Extract (and) BASF’s Nephoria (INCI: Maltodextrin (and) Nephelium Lappaceum
Octyldodecanol) from Ashland provides the soothing, calming and Leaf Extract) works to rejuvenate mature skin via biological
well-aging effects cannabidiol (CBD) oil is known for, without regula- pathways similar to retinol. It reportedly stimulates the formation
tory hurdles and controversy. It may also be used in sensitive skin of collagen and elastic fibers in order to help skin look
applications as it has anti-irritant and antiprutic properties. visibly younger.
NeoPlanta Withania
Evonik
www.evonik.com
Based on Ayurvedic naturals, Evonik’s
NeoPlanta Withania (INCI: Withania
Somnifera Root Extract (and) Glycerin
(and) Water (aqua)) is a multifunctional
active that reportedly protects skin
against premature aging caused by
stress and the environment, for a
smooth and healthy skin appearance.
HumaColl21
Geltor
Deodorant Active www.geltor.com
Created with zero animal inputs and
CareMagD via fermentation, Geltor’s HumaColl21
(INCI: Not Available) is a biodesigned
Clariant
collagen for cosmetics that offers im-
www.clariant.com proved skin collagen content, wrinkle
CareMagD (INCI: Magnesium Hydroxide reduction, firming and tightening with
(and) Magnesium Carbonate Hydroxide) improved elasticity and moisturization.
from Clariant is based on marine salts
to reportedly curb body odor in natural
deodorant formulations without the use of
aluminum. It leaves a dry, velvety skin feel
and absorbs excess sweat and sebum that
could otherwise become malodorous.
CT1905_Tech_Launches_fcx.indd 14 4/16/19 4:25 PM

Product Roundup [Ingredients, Equipment & Services]
Antioxidant and Probiotic Solutions
Antioxidant Standards
MilliporeSigma
Campo D.M.A.E. 99.99% www.SigmaAldrich.com
Campo Research The use of antioxidant standards is vital to ensuring the safety
www.campo-research.com and performance of a cosmetic product that incorporates
Dimethylaminoethanol Tartrate (DMAE) (INCI: Dimethylami- antioxidants. MilliporeSigma's standards manufacturing sites
noethanol Tartrate) is a natural organic compound, extracted are accredited to ISO/IEC 17025, ISO Guide 34 and ISO 17034,
from Mexican Skin Tree (Mimosa Tenuiflora). Campo D.M.A.E. which are the highest levels of quality achievable for reference
99.99% is a natural plant isolated metabolite of clear, pale- material producers.
yellow semisolid paste. It has amphiphilic properties as the
ingredient is, in behavioral aspects, comparable to how the
true DMAE exists in nature.
InfraGuard
Mibelle AG Biochemistry
www.mibellebiochemistry.com
InfraGuard (INCI: Caesalpinia Spinosa Fruit Pod Extract/Caesal-
HyWhite
pinia Spinosa Fruit Extract (and) Helianthus Annuus (Sunflower)
Contipro a.s. Sprout Extract (and) Propylene Glycol (and) Phenoxyethanol
www.contipro.com (and) Sodium Benzoate (and) Water (aqua)) combines tara tan-
HyWhite (INCI: Sodium Hyaluronate (and) Linolenic Acid) is a nins with organic sunflower sprouts to efficiently protect skin
derivative of a low molecular weight hyaluronic acid and cells from oxidative stress caused by infrared/blue light and
α-linolenic acid. Both parts of the molecule significantly particulate matter. InfraGuard neutralizes free radicals almost
contribute to the efficacy of the final product HyWhite. as efficiently as vitamin C. It scavenges 100% of ROS induced
Effectiveness was shown in both Asian and Caucasian skin by infrared inside the mitochondria, protecting cellular DNA
types, with a 40% improvement in skin lightness (ITA). and functions.
CT1905_Roundup_fcx.indd 15 4/16/19 4:32 PM

Market Intelligence | C&T ®
KEY POINTS
• Sagging is a complex phenomenon involving
changes in the dermis, subcutaneous fat
tissue and muscular changes.
• The present article reviews research related

to this phenomenon and topical approaches
to address it.
Consumer Perspective
Picking Up the Slack

Sagging Skin as an Anti-aging Target
Katerina Steventon, Ph.D.

FaceWorkshops, LLC,
Yorkshire, U.K.
16 | www.CosmeticsandToiletries.com
A ging forces changes to the facial shape
to become more apparent. To avoid the
surgery required to address skeletal
changes, formulators and consumers
alike have changed their focus to a new
anti-aging target—sagging skin.
Most research in skin sagging has been conducted in Japan.
One study1 confirmed that around the age of 40, Japanese
women experience reduced volume in the upper face and
Reproduction in English or any other language of

all or part of this article is strictly prohibited.
© 2019 Allured Business Media.
Vol. 134, No. 5 | May 2019
CT1905_Mrkt_Steventon_fcx.indd 16 4/23/19 11:17 AM

Product Development Workshop
Innovation Showcase
Curated Networking
October 15, 2019

New York, New York
www.beautyaccelerate.com
Produced by In Partnership with
Beauty_Accelerate_FP_CT.indd 1 3/19/19 12:46 PM

Picking Up the Slack
and positively to the elastic recovery from

deformation at the cheek area. Furthermore, a
Interactions between comparison of the anchor structures between
people in their 20s and 70s revealed a loss of
the dermis and anchors, eventually causing the sagging we see
with aging.5, 6
subcutaneous fat are Recently, further noninvasive magnetic
resonance imaging confirmed the density of
of interest to sagging. the fibrous network of retinacula cutis (RC)
structures in subcutaneous tissue correlates
negatively with sagging score and positively
with elasticity. These fibers are not uniform
across the face but vary in orientation and
increased volume in the cheeks and around the density across anatomical features; it is likely
chin, including the jawline.1 Until then, sagging that a sparse RC structure contributes to a
in the nasolabial groove is more noticeable, reduction in elasticity, resulting in a greater
and the mouth-corner area becomes prominent degree of sagging.7
thereafter, when sagging in the cheeks trans- Nasolabial folds are related, well-known
fers to the areas around the mouth.2 features of sagging and aging. They affect
Compared with Japanese populations over the subcutaneous adipose tissue that lies just
the age of 40, sagging is significantly higher in beneath the dermal layer. As individuals reach
Caucasians; indeed, Caucasian women seem middle age, the severity of their nasolabial
to have a higher susceptibility to sagging in folds increase, with decreased dermal elasticity
the subzygomatic area.3, 4 Regardless, sagging and an increased subcutaneous adipose layer.
represents a familiar concern to many, as it These changes could also induce sagging in
loosens facial definition; appears as droop- the upper cheek area, promoting fold forma-
ing at the corners of the eyes; and deepens tion at the border between the inner and outer
nasolabial lines. nasolabial areas.8
Interactions between the dermis and sub-
Causes of Sagging cutaneous fat are also of interest to cheek-area
Sagging is a complex phenomenon involv- sagging. The thickness of the subcutaneous
ing changes in the dermis, subcutaneous fat adipose layer impacts dermal elasticity
tissue and muscular changes; a loss in skin and sagging severity at the lower cheek. An
elasticity alone is insufficient to explain it. increased subcutaneous adipose mass impairs
While all factors that contribute to sagging dermal elasticity, which, in turn, exacerbates
and changes in the internal structure of facial cheek sagging.9
skin have yet to be fully elucidated, Japanese In an individual’s 40s, sagging of the cheeks
research has attempted to shed light on a seems to be associated with the reduction of
number of mechanisms. skin elasticity and mimetic muscle function.
For one, facial skin has been found to It is also linked to an increase in fat mass, but
contain convex, protruding structures under- it is important to note that this relationship is
neath the dermal layer. Through detailed different in various areas of the cheeks.10
analysis of these structures, researchers found
these collagen and elastin fibers are aligned Anti-sagging Technologies
vertically, whereas they are spread horizontally While topical products have aimed to
in the dermis. This suggests the protruding improve facial sagging, achieving clinical
“anchor” structures are responsible for holding efficacy within the described multifactorial
the skin in place through vertical elasticity. environment has not been easy. Shiseido R&D,
Aging causes these structures to slacken, for one, has been working to utilize its
thereby weakening the skin support and research into the mechanisms of facial skin
increasing sagging. structural changes and sagging to develop new
The depth of these structures relates nega- skin care products. They have demonstrated
tively to the elasticity and severity of sagging, that sagging can be offset by facial exercises or
CT1905_Mrkt_Steventon_fcx.indd 18 4/16/19 5:24 PM

ingredients such as licorice extract, which can 4. Wikipedia (Accessed 2019, Mar. 15). Zygomatic
bone. Retrieved from https://en.wikipedia.org/wiki/
reportedly mimic the effect of facial exercise Zygomatic_bone
and alleviate this concern.11 5. Shiseido (Accessed 2019, Mar. 15). Characteristic internal
Facial massage also has been shown to affect structure of the face contributes significantly to the face
subcutaneous fat tissues and facial expression aging factor = sagging. IFSCC Congress 2014, Paris,
Congress Poster Award. Retrieved from https://www.
muscles. Massage-induced morphological shiseidogroup.com/rd/ifscc/23.html
changes have been demonstrated by both digital 6. Ezure, T., Yagi, E., Amano, S., and Matsuzaki, K. (2016).
scanning and photography in the paranasal Dermal anchoring structures: Convex matrix structures
area, nasolabial fold area and cranial part of the at the bottom of the dermal layer that contribute to the
maintenance of facial skin morphology. Skin Res Technol,
mandibular area.12 22(2), 152-7.
Finally, a new concept developed by the 7. Sakata, A., Abe, K., Mizukoshi, K., Gomi, T., and Okuda, I.
Japanese company POLA is a serum focused (2018). Relationship between the retinacula cutis and sag-
on oxidized low-density lipoprotein (OxLDL), ging facial skin. Skin Res Technol, 24(1), 93-98.
which also targets facial sagging. OxLDL is said 8. Ezure, T., and Amano, S. (2012). Involvement of upper
cheek sagging in nasolabial fold formation. Skin Res Tech-
to stimulate subcutaneous adipocytes to secrete nol, 18(3), 259-64.
adipocytokine 4-1BB in the skin, which sup- 9. Ezure, T., and Amano, S. (2010) Influence of subcutaneous
presses the mRNA expression of RC-composing adipose tissue mass on dermal elasticity and sagging sever-
proteins. This, in turn, weakens RC structures ity in lower cheek. Skin Res Technol, 16(3), 332-8.
in skin tendon cells, resulting in facial sagging. 10. Ezure, T., Hosoi, J., Amano, S., and Tsuchiya, T. (2009).
Sagging of the cheek is related to skin elasticity, fat mass
This strategy therefore aims to reduce the secre- and mimetic muscle function. Skin Res Technol, 15(3),
tion of 4-1BB from skin adipocytes to facilitate 299-305.
the prevention of facial sagging. Therefore, 11. Ezure, T., and Ochiya, T. (2018, Feb. 2). Fat stem cell
targeting the modulation of adipocytokines attractant-containing agent for improving skin loose-
ness or aging caused by dermal cavitation. US Pat
could result in the development of new skin- US20180200179A1. Retrieved from https://patents.google.
sagging prevention products.13 com/patent/US20180200179A1/en
12. Nishimura, H., Okuda, I., Kunizawa, N., Inoue, T., Nakajima,
Y., and Amano, S. (2017). Analysis of morphological
References changes after facial massage by a novel approach using
1. Kurosumi, M., and Mizukoshi, K. (2018, May). Principal three-dimensional computed tomography. Skin Res Technol,
component analysis of three-dimensional face shape: 23(3), 369-375.
Identifying shape features that change with age. Skin Res 13. http://www.iloveweb.kr/IFSCC2017/file/Full_paper/Full%20
Technol, 24(2), 213-222. Paper%20P-049.pdf
2. Tsukahara, K., Takema, Y., Fujimura, T., Moriwaki, S.,
Kitahara, T., and Imokawa, G. (2000, Aug.). Determination
of age-related changes in the morphological structure (sag-
ging) of the human cheek using a photonumeric scale and
three-dimensional surface parameters. Int J Cosmet Sci,
22(4), 247-58. C&T Digital Edition
3. Tsukahara, K., ... Takema, Y., et al. (2004). Comparison of Get the latest in Cosmetics & Toiletries
age-related changes in wrinkling and sagging of the skin in digital edition exclusives every month!
Caucasian females and in Japanese females. J Cosmet Sci,
55(4), 351-71. http://www.CosmeticsandToiletries.com/DE
CT1905_Mrkt_Steventon_fcx.indd 19 4/17/19 11:33 AM

Regulatory | C&T ®
KEY POINTS
• Safety is a major consideration when

developing cosmetic products.
• This article describes safety guidelines in

the U.S. and EU, along with the steps to
take during development to ensure that
products are safe for human use.
Back to Basics
Part II Ensuring Product Safety
Editor's note: This series serves as a primer for the cosmetic development process. This second installment covers
C
product safety considerations in both the EU and U.S.; the first described crucial regulatory details. The next installment,
on microbiological considerations, will appear in the September issue of Cosmetics & Toiletries.
Pascal Yvon
BioSciences Expansion, LLC,
osmetic product safety for human health
Newtown, PA U.S.
is a must. The European Commission (EC)
Regulation and the Federal Food, Drug,
and Cosmetic Act (FD&C Act) in the U.S.
require cosmetic products to be safe for
human health, outlined as follows.
Disclaimer: Check with your regulatory specialist to review your specific product and situation.

20 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 134, No. 5 | May 2019
CT1905_Regulatory_Yvon_fcx.indd 20 4/16/19 4:51 PM

• EU: The EU states, "A cosmetic product
made available on the market shall be
safe for human health when used under
normal or reasonably foreseeable condi-
Choosing ingredients
tions of use."1 from organic or
• U.S.: The U.S. prohibits the marketing
of adulterated or misbranded cosmetics. natural sources is no
A cosmetic is considered adulterated if,
"It bears or contains any poisonous or guarantee of safety.
deleterious substance which may render
it injurious to users under the conditions
of use prescribed in the labeling thereof,
or under conditions of use as are custom-
ary and usual."2
Manufacturers are responsible for ensuring A reported 50% of skin care consumers say
the safety of their products, along with they are currently seeking products that claim
safety substantiation. to be all-natural or free-of synthetic chemicals.
In Europe, the safety of cosmetic products is
based on the safety of the ingredients within—
this includes their toxicological profile and
exposure level. The rationale behind this comes Source: Future Market Insights
from the fact that many thousands of different

Back to Basics, Part II
products are all derived from a limited number In vitro tests and testing strategies to address
of substances. the various endpoints have been developed and
Europe’s regulations prohibit the marketing validated.3 These studies must be performed
of finished products containing ingredients that in a GLP-certified laboratory. When sourcing
have been subject to animal testing since March for ingredients, it is important to collect their
2013, as notified in (EC) 1223/2009 Art. 18.1 safety data from the suppliers. Also, possible
Animal testing in cosmetics has been banned interactions between ingredients in the final for-
in many other countries as well, with new mulation, with potential safety relevance, should
and similar regulations currently in the works be considered. Endpoints that may be relevant
around the world and in multiple U.S. states. to consider for the final formulation include:
• Skin irritation;
Testing for Safety • Eye irritation; and
The safety of ingredients is evaluated by • Skin sensitization.
toxicological testing. Endpoints that may be
For skin sensitization, the Human Repeat
relevant for the toxicological profile of
Insult Patch Test (HRIPT) often is used. It com-
ingredients include:
prises a clinical study of a panel of volunteers
• Skin and eye irritation; to assess the sensitizing potential of the product
• Skin sensitization; after repeated applications. For ethical reasons,
• Genotoxicity; and the HRIPT can only be performed if induction
• Photo-induced
toxicity.
(EC) 1223/2009 Key Considerations
Annex I indicates
• The safety of cosmetic products for human health is a must.
that “a particular
focus on local toxicity • All physicochemical properties and information on the impurities about each
evaluation (skin and ingredient must be collected for safety assessment.
eye irritation), skin • Plan the budget and time for testing to appropriately validate safety to consumers.
sensitization, and
• Conduct some toxicological/tolerance testing with the complete formulation.
in the case of UV
absorption, photo- • In some territories (e.g., EU), a dossier must be drawn up with a safety assessment
induced toxicity shall established by a qualified professional.
be made.”1

Figure 1. EU product information file and cosmetic product safety report
is not expected based on the available pre- assessment of the product, while Part B sets out
information; i.e., the toxicological profile review the reasoning for drawing conclusions as to the
of each ingredient and its clinical final security safety of the product.
test. Within the scope of the EC, the HRIPT
should be used as a confirmation test,
only to demonstrate the absence of
sensitization potential.
Manufacturers
are responsible for
ensuring the safety
of their products,
along with safety
substantiation.
In order to demonstrate that a cosmetic

product complies with (EC) 1223/2009 Art. 3, it
must have undergone a safety assessment on the
basis of the relevant information and a cosmetic
product safety report must be set up in accor-
dance with Annex I (Art. 10). This safety report
is a component of the Product Information
File and comprises two parts (see Figure 1).
Part A aims to gather all the data for the safety

Back to Basics, Part II
Part A lists the minimal data that must be made

available, which includes:
• The quantitative and qualitative composition of
the cosmetic product;
• Physical/chemical characteristics and stability of
the cosmetic product;
• Microbiological quality and results of preserva-
tion challenge tests;
• Impurities, traces and information about the
packaging material;
• Normal and reasonably foreseeable use;
• Exposure to the cosmetic product;
• Exposure to the substances contained therein;
• Toxicological profile of the substances;
• Undesirable effects and serious undesirable
effects; and
• Information on the cosmetic product.
Adulterated Cosmetics
In the U.S., adulteration refers to violations involv-
ing product composition, whether as a result of
ingredients, contaminants, processing, packaging or
shipping and handling.
A cosmetic is adulterated if:
• As noted above, it bears or contains any poison-
ous or deleterious substance which may render
it injurious to users under the conditions of
use prescribed in the labeling thereof, or under
conditions of use as are customary and usual
(with an exception made for coal-tar hair dyes);
• It consists in whole or in part of any filthy,
putrid or decomposed substance;
• It has been prepared, packed or held under
unsanitary conditions whereby it may have
become contaminated with filth, or whereby it
may have been rendered injurious to health;
• Its container is composed, in whole or in part,
of any poisonous or deleterious substance which
may render the contents injurious to health; or
• With the exception of coal-tar hair dyes, it is, or
it bears or contains, a color additive which is
unsafe within the meaning of section 721(a) of
the FD&C Act.
The U.S. Food and Drug Administration (FDA)
has consistently advised manufacturers to use what-
ever testing is necessary to ensure the safety of their
products and ingredients. Although U.S. regulations
do not currently specify particular testing regimens
for cosmetic products or ingredients, the cosmetic
company is responsible for substantiating product
and ingredient safety prior to marketing. The FDA has
advised that:

“...the safety of a product can be adequately in cosmetics in the U.S. The available assess-
substantiated through (a) reliance on already ments can be accessed via the CIR websitea.
available toxicological test data on individual Finally, as is well-known, choosing ingredients
ingredients and on product formulations that from organic or natural sources is no guarantee
are similar in composition to the particular that they are safe—in the end, manufacturers are
cosmetic, and (b) performance of any additional still responsible for making sure their products
toxicological and other tests that are appropriate meet safety requirements.
in light of such existing data and information.
Although satisfactory toxicological data may exist References
for each ingredient of a cosmetic product, it will 1. Regulation (EC) No 1223/2009 of the European Parliament
still be necessary to conduct some toxicological and of the Council. (2009). Retrieved from https://ec.europa.
testing with the complete formulation to assure eu/health/sites/health/files/endocrine_disruptors/docs/
cosmetic_1223_2009_regulation_en.pdf
adequately the safety of the finished cosmetic.”4
2. Federal Food, Drug, and Cosmetic Act (FD&C Act). Retrieved
It must also be noted that, according to the from https://www.fda.gov/regulatoryinformation/lawsenforced-
Code of Federal Regulations:5 byfda/federalfooddrugandcosmeticactfdcact/default.htm
“Each ingredient used in a cosmetic product 3. P. Yvon, P. (2015). Market your cosmetics in Europe with
and each finished cosmetic product shall be safety. Happi, 66-69.
adequately substantiated for safety prior to 4. Food, Drug, And Cosmetic Products, 40 Fed. Reg. 8916
(March 3, 1975). Retrieved from https://www.loc.gov/item/
marketing. Any such ingredient or product whose fr040042/
safety is not adequately substantiated prior to 5. Labeling of cosmetic products for which adequate sub-
marketing is misbranded unless it contains the stantiation of safety has not been obtained. Retrieved from
following conspicuous statement on the principal https://www.accessdata.fda.gov/scripts/cdrh/cfdocs/
cfcfr/CFRSearch.cfm?fr=740.10
display panel:
‘Warning—The safety of this product has not
been determined.’”
a
www.cir-safety.org
Conclusion
A resource for the manufacturers is the
C&T Online
Cosmetic Ingredient Review (CIR) program. The
For more on CIR rulings, check out our "CIR Conclusion"
CIR expert panel is an independent, nonprofit column by Bart Heldreth, Ph.D., executive director of the CIR,
scientific body established in 1976 to thoroughly on www.CosmeticsandToiletries.com.
review and assess the safety of ingredients used

Research | C&T ®
KEY POINTS
• The profiles of the biological actives in
rice differ during grain development;
they are particularly high during the
flowering phase.
• Here, a flowering jasmine rice panicle
extract was tested for skin benefits
and proven to be a safe and effective
anti-aging active.
Mayuree Kanlayavattanakul, Nattaya Lourith, Ph.D.
and Puxvadee Chaikul
Mae Fah Luang University, Thailand
Youth in Yields
Jasmine Rice Extract Whitens, Protects and Smooths Skin
T he demand from
consumers for natural
products—including
cosmetics—con-
tinues to increase.
Eco-friendly,
organic and sustainable options are in the
mainstream of this trend. Moreover, active
phenolics derived from natural sources are
playing an important role in the safety and
efficacy of cosmetics.1
In relation, rice, or Oryza sativa cv.
particularly high during the flowering phase
between 0-7 days of the development, during
which the panicle, or cluster of branches,
is still green. Flowering rice panicle was
therefore explored, as described next, for
applications as an eco-friendly, sustain-
able, safe and efficient active ingredient
for cosmetics.2-4
Furthermore, beneficial integration
between cosmetic manufacturers and the
farmers who grow the active ingredient
plants provides an opportunity to improve the
by farmers whose incomes heavily rely
upon rice cultivation.
Materials and
Methods
Rice panicle extract: The rice
panicles of five different varieties
cultivated in Chiang Rai were harvested;
two glutinous rice varieties and three
longer grain organic white rice. The
harvested rice panicles were treated and
prepared by a method developed to yield
indica (Oryzeae), is well-known as the major local quality of life, giving would-be cosmetic phenolic-rich extracts.2-4
staple in Asian cuisine. It has long been consumers a path toward goodwill. The Total phenolics content (TPC): The
used in traditional Asian medicines as well present work relates to rice farmed in Chiang TPC of each extract was comparatively
as Italian remedies, including for aesthetic Rai, the northernmost province in Thailand, analyzed by Folin-Ciocalteu assay.2-4
benefits for skin. located in the renowned Golden Triangle Phenolics analysis: The content of
The profiles of the biological actives in area. Home to majestic mountains and the cosmetic active phenolics was
rice differ during grain development and are breathtaking waterfalls, this area is inhabited analyzed by the validated

26 | www.CosmeticsandToiletries.com language ofallallororpart
Reproduction in English or any other partofofthis
thisarticle
articleisisstrictly
strictlyprohibited. Media.134, No. 5 | May 2019
prohibited. © 2019 Allured Business Vol.
CT1905_Rsrch_Lourith_fcx.indd 26 4/16/19 5:01 PM


Youth in Yields
p -Coumaric and ferulic acids, along with 10

additional minor phenolics, were identified as
the extract's major active constituents.
ultra-performance liquid chromatography proteins-2 (TRP-2) were assessed at the safe

(UPLC) method;5 particularly gallic (GA), extract concentration.5
protocatechuic (PA), chlorogenic (ChA), caffeic Rice panicle cream development: A base
(CA), syringic (SyA), p-coumaric (pCA), ferulic and test cream containing (or not) the rice
(FA), sinapic (SiA) and rosmarinic (RA) acids; panicle extract, (see Formula 1) was developed
as well as vanillin (V) and quercetin (Q). and physicochemically evaluated. It stability
In vitro antioxidant activity: The extracts also was tested by means of a centrifugation
were assessed for antioxidant activity in vitro assay and seven heat-cool cycles.3, 5
by 2, 2'–azino-bis(3-ethylbenzothiazoline)-6-sul- Clinical evaluations: Finally, a study
fonic acid (ABTS), 1,1-diphenyl-2-picrylhydrazyl protocol following the guidelines of the Declara-
(DPPH) and ferric reducing ability of tion of Helsinki and Tokyo was approved by the
plasma (FRAP) assays and compared with ethics committee of Mae Fah Luang University.
the standards.2-4 Primary skin irritation tests were performed
In vitro enzyme inhibitory effects: The in 25 subjects by a single application, closed-
inhibitory effect of the extracts against mush- patch test for 24 hr on the volar forearms of
room tyrosinase was assessed as per elastase the subjects. Skin irritation severity was graded
and collagenase (see Figure 1).2-4 from 0-4 to calculate the Mean Irritation Index
Properties and stability: The solubility of (MII). A MII < 0.2 was interpreted as non-
the extract was examined in different cosmetic irritating. The base and rice panicle creams
vehicles, whose appearance and physicochemi- were examined in parallel with 0.5% sodium
cal properties were recorded prior to stability lauryl sulfate (positive control) and water (the
testing under accelerated conditions.2, 3 negative control).
Activity in human skin fibroblasts: The A randomized, double-blind, placebo-
extract safety profile was investigated, and controlled efficacy study was conducted in 24
antioxidant activity of the extract was analyzed healthy volunteers who applied the samples
in fibroblasts at the safe dose.5 twice daily (morning and evening). The treated
Activity in B16F10 melanoma cells: The skin was evaluated for characteristics such as
cytotoxicity of the extract in melanoma cells hydration levelsa, elasticityb, melanin and erythe-
was examined. Inhibitory effects against mac, and surface topographyd at the baseline
melanogenesis, tyrosinase and tyrosinase related and after 2, 4, 8 and 12 weeks of treatment.3, 5
Statistical analysis: The measured param-
eters were compared and analyzed using one
sample t test and ANOVA test, with a signifi-
cance level of p < 0.05 using softwaree.
The global anti-aging market, including
cosmetics, services and devices, is expected Results: In vitro
to expand at a CAGR of 5.73% between 2018 As noted, a concise technique,2, 3 which is
and 2023, and reach $429 billion by 2022. feasible for industrial scaling, was developed
a
Corneometer CM 825,
Source: Mordor Intelligence
b
Cutometer MPA 580,
c
Mexameter MX 18 and
d
Visioscan VC 98, are devices from Courage & Khazaka.
e
SPSS program version 16.0, IBM

and used to extract the rice panicle actives to could be used as a feasible method for the qual-
yield phenolic-rich extracts. The active constitu- ity control of the extract (not shown).3
ents of the extracts were quantified and jasmine The safety profile and activity of the extract
rice, or Khao Dawk Mali 105 (ML), exhibited in cell cultures of human skin fibroblasts and
the best TPC and in vitro antioxidant activities B16F10 melanoma also were observed. The
(see Table 1). p-Coumaric and ferulic acids extract demonstrated no cytotoxicity to human
were determined through UPLC analysis to be skin fibroblasts or B16F10 melanoma cells at a
the major extract components, along with the maximum dose of 0.1 mg/mL. The extract was
presence of 10 minor phenolics. additionally shown to protect the cell from oxi-
Radical-scavenging phenolics are common dative stress at doses of 0.1 mg/mL or lower, as
in anti-aging product formulations, and they per its major phenolics, p-coumaric and ferulic
additionally exhibit enzyme inhibitory effects. acids (see Figure 2), similar to the standard,
Tyrosinase is known as the melanogenesis vitamin C.5 In addition, cells treated with the
enzyme, whereas elastase and collagenase are ML extract (0.1 mg/mL) suppressed melanogen-
matrix metalloproteinases (MMPs), which esis via tyrosinase (tyr) and TRP-2 inhibitory
degrade elastin and collagen, skin-firming fibers. effects. In fact, the rice panicle extract and its
Testing against these enzymes will therefore major constituents, p-coumaric and ferulic
guide the potency of the active constituents to acids, were shown to be more potent at reducing
combat skin aging.1 melanin content levels than KA (see Figure 3).
The antioxidant activity of the ML
extract (0.4 mg/mL) against mushroom tyrosi-
nase was lower than the kojic acid control Formula 1. Test Jasmine Rice
(KA, 0.2 mg/mL). However, its anti-elastase Panicle Cream
activity (0.08 mg/mL) was better than the
standard p-coumaric acid (0.04 mg/mL) and Acrylates/C10-30 Alkyl Acrylate Crosspolymer
comparable to ferulic acid (0.04 mg/mL); (Carbopol Ultrez-21, Lubrizol)
although less potent than ursolic acid (UA). In Water (aqua)
addition, the rice panicle extract (0.1 mg/mL) Propylene Glycol
possessed anti-collagenase activity comparable 4 Sodium EDTA
to the standard epigallocatechin gallate (EGCG), Cyclomethicone (Dub 165, DuBois)
tested at 0.05 mg/mL (not shown).3, 5 Shea Butter
Prior to safety and biological activity Stearic Acid
assessments of the ML extract in cell cultures, Rice Bran Oil
its stability was examined. The extract was TEA 99%
found to be physicochemically and chemically Vitamin E Acetate
stable following accelerated stability tests. Total Propylene Glycol (and) Diazolidinyl Urea (and)
phenolic content was reduced by 5.37 ± 0.24%, Iodopropynyl Butylcarbamate
as per UPLC analysis, of which p-coumaric acid (Liquid Germal Plus, Ashland)
was 7.33 ± 0.17%, reduced in harmony with the Rice Panicle Extract
7.62% reduction of TPC. Thus, TPC analysis
Table 1. Phenolic Content and Antioxidant Activities of Jasmine Rice Panicle Extract
Active constituent TPC Not less than 23 g GAE/100 g

pCA Not less than 3,500 μg/mL
FA Not less than 600 μg/mL
In vitro antioxidant activity ABTS (at 100 ppm) Not less than 80%
DPPH (at 400 ppm) Not less than 90%
FRAP (EC at 1 mg extract) Not less than 490 μg FeSO4

Youth in Yields
Thus, the anti-melanogenesis benefits of the ensured. The biological properties of the
rice panicle extract were proven by its abilities ML extract were also confirmed in vitro and
to suppress the tyrosinase and TRP-2 enzymes ex vivo, as described; as such, the extract
(see Figure 3).5 was next developed into a cosmetic cream to
Overall, quality control, standardization confirm its physicochemical properties and
and stability of the extract were therefore chemical stability.3, 5
Figure 1. In vitro enzyme inhibitory activities of the rice panicle extract in a comparison with
standards
Figure 2. Safety and antioxidant activity of the rice panicle extract in human skin fibroblasts, in
comparison with standards

The jasmine rice panicle extract cream
increased skin hydration, brightness,
firmness and smoothness.
Results: In vivo treatment.5 Finally, the degree of skin wrinkling

The rice panicle creams (ML creams), includ- was significantly reduced; skin smoothness was
ing 0.1% and 0.2% of the extract, and the base significantly induced (p ≤ 0.004 and ≤ 0.038) by
cream showed no signs of skin irritation upon the ML creams after two months of treatment
topical exposure, similar to water (MII = 0). (see Figure 5).3, 5-7
Clinical efficacy evaluations were consequently
examined in seven male and 17 female volun- Conclusion
teers, aged 37.46 ± 6.66 years by a randomized, In summary, the concise extraction of rice
double-blind, placebo-controlled trial.3, 5-7 panicle actives, feasible for industrial scale,
ML-treated skin was significantly (p < 0.001) was developed and the active constituents of
lightened after four weeks of treatment, and the extracts were identified. Quality control,
both 0.1% and 0.2% ML creams were compara- standardization, stability, safety and biological
ble (p ≥ 0.622) in lightening efficacy. ML cream activities of the extract were ensured, as per
treatment for 4-12 weeks also significantly the extract’s compatibility with other cosmetic
(p < 0.05) improved skin moisture levels better ingredients.2, 3, 5
than two weeks of treatment (see Figure 4).3, 5-7 Next, a cosmeceutical cream containing
Following one month of treatment, the ML jasmine rice panicle extract was shown to effec-
creams significantly (p ≤ 0.045) increased skin tively increase skin hydration within two weeks;
firmness (Ur/Uf) relative to the cream base, and skin brightness and firmness within four weeks;
this firmness was enhanced by longer periods of and skin smoothness within eight weeks.3, 5-7 The

Youth in Yields
Figure 3. Anti-melanogenesis activities of the rice panicle extract in B16F10 melanoma cells,
in comparison with standards
Figure 4. Skin lightening and hydrating efficacies of the rice panicle cream evaluated in
human volunteers

Figure 5. Skin wrinkle-reducing, firming and smoothing efficacies of the rice panicle cream
evaluated in human volunteers
extract is therefore encouraged for cosmetic 5. Kanlayavattanakul, M., Lourith, N., and Chaikul, P. (2016).
Jasmine rice panicle: A safe and efficient natural ingredient
product applications in different dosage forms, for skin aging treatments. J Ethnopharmacol 193 607-616.
based on its presenting evidence-based efficacy. 6. Kanlayavattanakul, M., Lourith, N., and Chaikul, P. (2017,
Furthermore, the extract meets the cosmetic Nov. 30-Dec. 3). Lanadene jasmine rice age defying facial
consumer’s expectation for a safe and efficient, cream. Award for high scientific and technological level of
the invention. The Ministry of Education and Science of the
eco-friendly active. The sustainable utilization Russian Federation. The 13th Annual of Seoul International
of available agricultural crops by transforming Invention Fair (SIIF 2017) Coex.
the rice panicle—less than seven days before 7. Kanlayavattanakul, M., Lourith, N., and Chaikul, P. (2017,
the milky phase of rice development—into a Nov. 30-Dec. 3). Lanadene jasmine rice age defying facial
cream. Gold prize. The 13th Annual of Seoul International
cosmetic active can add a more than tenfold Invention Fair (SIIF 2017) Coex.
value to rice grain. Thus, the presented cosmetic
active would not only benefit cosmetic users,
but the farmers who grow rice, improving their
quality of life.
C&T Digital Edition

References
Get the latest in Cosmetics & Toiletries
1. Kanlayavattanakul, M., and Lourith, N. (2015). An update digital edition exclusives every month!
on cutaneous aging treatment using herbs. J Cosmet Laser
Ther 17343-352.
http://www.CosmeticsandToiletries.com/DE
2. Thai Patent No. 138486 (2013, Dec. 19). Assigned to Kan-
layavattanakul, M., Lourith, N., and Tadtong, S. Preparation
of rice panicle extract for utilization in health promotion and
cosmetic products. Int Cl 10 A61K 36/899, A61K 8/97.
3. Thai Patent No. 11045 (2015, Mar. 6). Assigned to Kanlaya- C&T Daily Newsletter
vattanakul, M., and Lourith, N. Manufacturing process of
rice panicle extract. Int Cl 10 A61K 35/00. Get the latest from Cosmetics & Toiletries
4. Kanlayavattanakul, M., Lourith, N., Tadtong, S., and Jon- delivered straight to your inbox every day!
grungruangchok, S. (2015). Rice panicles: New promising
unconventional cereal product for health benefits. J Cereal http://www.CosmeticsandToiletries.com/newsletter
Sci 66 10-17.

Testing | C&T ®
KEY POINTS
• When collagen breaks down,
the broken fragments can hinder
the performance of anti-aging
actives over time.
• This column examines methods
by which materials can overcome
these aging-related issues in
collagen production.
Testing Tactics in Skin
Total Breakdown
Y
Recovering Anti-aging Efficacy After Collagen Fragmentation
Robert Holtz
BioInnovation Labs, Inc. ou may have heard of King Arthur, with his
Denver, U.S. interminable search for the holy grail. In one
film renditiona, the secret of the grail is sim-
ply that the land and Arthur are one. As one
thrives, so does the other and, unfortunately,
as one suffers the other suffers as well. It is a
wonderful illustration of interdependence, in which changes to one
partner in a relationship can significantly impact the other.
a
Excalibur, 1981

CT1905_Testing_Holtz_fcx.indd 34 4/16/19 5:11 PM

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Possesses Robust Dual Inhibitory Activity Against Oxidative & Inflammatory Stress
HydraSynol™ IDL (INCI: Isosorbide Disunflowerseedate):

Reduces & Repairs Skin Barrier Dysfunction via Multiple Pathways
SYTHEON LTD. • 315 Wootton Street, Boonton, NJ 07005 • www.sytheonltd.com • info@sytheonltd.com • Tel.: +1 973.988.1075
SYTHEON SARL • 112 rue de Paris, 92100 Boulogne Billancourt • www.sytheonltd.com • sytheon@sytheonltd.com • Tel.: +33 (0)1.4110.8182

Total Breakdown
Collagen fragmentation is a slowly occurring

but nonetheless inevitable degradation
associated with both chronological aging
and photoaging.
What does any of this have to do with skin and the ECM component makes its way into the
care? Quite a bit, when you closely examine the ECM—end of process.
interrelationship between the dermal layer of This is essentially how it works in most
the skin and its main constituent cell type—the in vitro experiments, and it is a good model to
dermal fibroblast. screen for in vivo efficacy in younger individu-
The dermal layer of the skin consists of als. However, the process becomes vastly more
densely packed extracellular matrix (ECM) complicated with both chronological aging and
components, such as collagen and elastin pro- sun exposure. Under these conditions, the ECM
teins, which provide the structural strength and becomes damaged, and this damage in the ECM
elasticity to skin; alongside glycosaminoglycans, can have a feedback effect on the fibroblast. This
proteoglycans and glycoproteins. Of all of these can produce drastic and adverse consequences
components, collagen is by far the most abundant on the fibroblast, such as stimulating an
and comprises about 90% of the skin’s dry weight, increase in MMP production; shutting down col-
with type I collagen being the predominate type.1 lagen synthesis pathways; and even driving the
As is well-understood, the main source of fibroblast into an early senescence.2 In essence,
production for all of these ECM components is the damaged ECM signals the fibroblast to not
dermal fibroblasts, with the rate of production only shut down the pathways responsible for
controlled by various hormonal, autocrine, para- synthesizing the ECM components, but also to
crine and physical factors. Indeed, increasing the become unresponsive to any stimuli that would
production of these ECM components is one of turn these pathways back on. This list of stimuli
the main targets for cosmetic active ingredients, could potentially include cosmetic actives,
as the inevitable reduction in their production, in which case the efficacy of an active could
e.g., due to aging and sun exposure, is associated decline as the age of the user increases.
with the undesirable fine lines and wrinkles, as So what is the type of ECM damage associ-
well as sagging and thinning skin, which drives ated with these adverse effects on fibroblasts?
our industry. Unfortunately, though, the focus And can it be prevented or countered?
is too often targeted on the fibroblast alone as
experiments are planned. We assume the process Collagen Fragmentation
flows in a single direction: active ingredients One of the more prominent forms of ECM
stimulate the fibroblast and in return, the fibro- damage occurring with aging and sun exposure
blast makes more of the target ECM component is collagen fragmentation. The initial driving
mechanism is thought to be caused by ROS
formation.3 With chronological aging, intracel-
lular ROS formation occurs slowly but steadily
Creams and moisturizers are the most popular
over time as a result of normal cellular func-
anti-wrinkle products; the growing anti-
tions, such as mitochondrial metabolism. In
wrinkle market is expected to reach
contrast, ROS formation can be rapidly and
$12.8 billion by 2027.
quite significantly increased with UV expo-
sure. Unfortunately, the skin that undergoes
Source: Future Market Insights both chronological aging and is exposed to
UV can experience the additive effect of both
ROS sources.

In response to the ROS, dermal fibroblasts
will decrease their production of collagen and
increase their production of MMP1. MMP1 is
essential to begin the process of collagen deg-
radation—it will cleave a single specific site in
the collagen fibril, which then opens up access
to other MMPs, i.e., MMP3 and MMP9—to
further degrade the collagen fibril.4 However, the
areas where collagen is covalently cross-linked
with other collagen fibrils
are highly resistant to
enzymatic degrada-
tion; therefore, these
small leftover collagen
fragments in cross-
linked areas cannot be
removed and are, for
all practical purposes,
permanently left in the
ECM where they accumulate
over time.
In addition to the effects on
MMP1 production, exposure of
dermal fibroblasts to ROS will
decrease collagen production. This
limits the replacement of collagen
that was excised through MMP
activity and leads to an imbalance
between collagen breakdown and
collagen synthesis, favoring a net
VIDEO
loss of collagen over time. Also, due
Hyaluronan Homeostasis
to the collagen fragments left in
the ECM by the incomplete break-
for Anti-aging Effects

down of collagen fibrils by MMPs,
what collagen is produced by the
fibroblasts is not deposited in an
organized manner.
While ROS may be responsible
for initially driving the collagen
fragmentation process, the process
unfortunately becomes self-sustain-
ing. Fibroblasts attach themselves
to the collagen fibrils of the ECM
in a manner similar to a spider
walking on its web. This contact is
mediated by integrins, transmem-
brane proteins that connect to the
ECM on the outside of the fibroblast
and to the actin cytoskeleton and
various second messenger systems
inside the fibroblast. As collagen
fragmentation increases, the
number of binding sites to which
CT1905_Testing_Holtz_fcx_DE.indd 37 4/23/19 11:22 AM

Total Breakdown
fibroblasts can attach within the collagen portion can be prevented by blocking integrin αVβ3,10
of the matrix decreases. These attachments to suggesting that the CCN1 pathway could be an
the ECM are important, as they apply a stretch attractive target for anti-aging actives.3
tension on the cell that is essential for normal
fibroblast function.5, 6 Without this tension on In vitro Models of
the fibroblasts, MMP production increases and Collagen Fragmentation
collagen synthesis pathways are shut down.3
To study the effects of fragmented collagen
Thus, the cycle of collagen fragmentation begins
on dermal fibroblasts, one of the main models
to perpetuate itself, slowly at first, but the rate
used in the literature is the collagen lattice.
of fragmentation will increase due to both the
Collagen lattices are essentially 3D collagen
accumulation of more and more collagen frag-
gels seeded with human fibroblasts—in other
ments and due to further exposure to ROS.
words, a simplified model of the dermal layer
of the skin. The collagen gel itself is typically
Mediator of Collagen prepared with type I collagen (rat tail collagen)
Fragmentation mixed with cell culture media, then pH-adjusted
The mechanism by which ROS formation and incubated to promote collagen polymeriza-
within fibroblasts induces an increase in MMP1 tion.11 After the collagen has polymerized, it can
production and decrease in collagen production be digested with MMP-1 to promote collagen
appears to be mediated in part by cysteine-rich fragmentation and then seeded with dermal
protein 61 (CCN1), a member of the CCN fam- fibroblasts. Fibroblasts cultured in collagen
ily of proteins.7, 8 CCN1 can be synthesized and lattices that have collagen fragmentation will
secreted by dermal fibroblasts, and its expression exhibit several traits associated with aged
and secretion by dermal fibroblasts is signifi- skin, such as increased intracellular ROS, an
cantly increased in both chronologically aged increased content of oxidized proteins, and
and photoaged skin.9 Once secreted, CCN1 can increased MMP-1 production.11 The fibroblasts
exert an autocrine/paracrine effect by binding to in this model may be more resistant to actives
integrins in the fibroblast membrane and activat- that promote collagen stimulation. Therefore,
ing intracellular pathways that increase MMP1 this type of model offers the ability to test
production and inhibit the pathways associated actives that are soluble in cell culture media in
with collagen production.2 The adverse effects a dermal environment that better mimics aged
of CCN1 on collagen metabolism in fibroblasts skin, and may give a better representation of

Unfortunately, the focus is too often targeted
on the fibroblast alone—the testing process
is more complicated in certain cases.
the in vivo efficacy of that active when compared the behavior found in aged skin (i.e., increased
with traditional monolayer cultures. MMP1 production and decreased collagen
Another model to assess the impact of actives production). With this model, decreases in type I
in aged skin suffering the effects of collagen collagen and increases in MMP1 can be observed
fragmentation are full thickness tissue modelsb. with CCN1 treatment,12 suggesting this may be
In contrast to the collagen lattice model, these an excellent in vitro model of aged skin for test-
skin tissue models possess both a dermal and ing topical applications.
epidermal layer. The dermal layer is essentially Finally, as CCN1 appears to be a major
the same as the collagen lattice described above; mediator of collagen fragmentation, simple cell
it is a type I collagen gel (nonfragmented) seeded culture monolayer studies can be conducted to
with human dermal fibroblasts. However, it also determine if actives can prevent CCN1 induction.
has a fully functional epidermal layer, which CCN1 expression in dermal fibroblasts appears
allows for the topical application of formula- to be initiated by ROS exposure. Simply treating
tions, allowing cosmetic actives to be applied in dermal fibroblasts in a monolayer culture with
an identical manner to which they would be used oxidants such as hydrogen peroxide or with
commercially. Since the dermal collagen in the UVB irradiation is enough to start the process of
full thickness tissue models is not fragmented, CCN1 production and secretion.7, 13 This simple
CCN1 can be added directly to the culture media in vitro model would be excellent for testing
to establish fibroblast behavior that is similar to actives, especially antioxidants, for their ability
to prevent CCN1 production as CCN1 production
b
i.e., Epiderm Full Thickness (EFT) model, MatTek

Total Breakdown
can be measured easily with commercially avail- 4. Overall, C. M. (2002). Molecular determinants of metal-
loproteinase substrate specificity: matrix metalloproteinase
able ELISA kits. substrate binding domains, modules, and exosites. Molecu-
lar Biotechnology, 22, 51-86.
Concluding Remarks 5. Cole, M. A., Quan, T., Voorhees, J. J., and Fisher, G. J.
Collagen fragmentation is a slowly occurring (2018). Extracellular matrix regulation of fibroblast function:
redefining our perspective on skin aging. Journal of Cell
but nonetheless inevitable degradation of the Communication and Signaling, 12, 35-43.
ECM associated with both chronological aging 6. Makhija, E., Jokhun, D. S., and Shivashankar, G. V. (2015).
and photoaging. This progressive damage not Nuclear deformability and telomere dynamics are regulated
only leads to both the cosmetic and pathological by cell geometric constraints. Proceedings from the National
Academy of Science, Supplement E32-E40.
changes associated with the ECM and aging,
7. Qin, Z., Robichaud, P., He, T., Fisher, G. J., Voorhees, J. J.,
but it also significantly impairs the function of and Quan, T. (2014). Oxidant exposure induces cysteine-rich
dermal fibroblasts and leads to fibroblasts that protein 61 (CCN1) via c-jun/AP-1 to reduce collagen expres-
are prematurely senescent and unresponsive to sion in human dermal fibroblasts. PLoS One, 9(12) e115402.
stimuli that could correct the adverse changes in 8. Lau, L. F., and Lam, S. C. (1999). The CCN family of angio-
genic regulators: The integrin connection. Experimental Cell
the ECM. Research, 248, 44-57.
Fortunately, there are in vitro models avail- 9. Quan, T., et al. (2006). Elevated cysteine-rich 61 mediates
able that can help to screen for actives to either aberrant collagen homeostasis in chronologically aged and
prevent or delay collagen fragmentation by photoaged human skin. American Journal of Pathology, 169,
482-490.
inhibiting the cycle of MMP1 production and
10. Qin, Z., Fisher, G. J., and Quan, T. (2013). Cysteine-rich
collagen synthesis inhibition, or by mitigating the protein 61 (CCN1) domain-specific stimulation of matrix
factors that can contribute to the loss of fibroblast metalloproteinase-1 expression through αVβ3 integrin in
human skin fibroblasts. The Journal of Biological Chemistry,
function, such as CCN1.
288(17), 12386-94.
11. Fisher, G. J., et al. (2009). Collagen fragmentation promotes
References oxidative stress and elevates matrix metalloproteinase-1 in
fibroblasts in aged human skin. The American Journal of
1. Uitto, J. (1986). Connective tissue biochemistry of the aging
Pathology, 174(1), 101-114.
dermis. Age-related alterations in collagen and elastin. Derma-
tological Clinics, 4, 433-446. 12. Quan, T., Qin, Z., Shao, Y., Xu, Y., Vorrhees, J. J., and Fisher,
G. J. (2011). Retinoids suppress cysteine-rich protein 61
2. Quan, T., and Fisher, G. J. (2015). Role of age-associated
(CCN1), a negative regulator of collagen homeostasis, in skin
alterations of the dermal extracellular matrix microenvironment
equivalent cultures and aged human skin in vivo. Experimen-
in human skin aging: a mini-review. Gerantology, 61, 427-434.
tal Dermatology, 20(7), 572-576.
3. Fisher, G. J., Sachs, D. L., and Voorhees, J. J. (2014). Ageing:
13. Quan, T., et al. (2010). Ultraviolet irradiation induces CYR61/
collagenase-mediated collagen fragmentation as a rejuvena-
CCN1, a mediator of collagen homeostasis, through activa-
tion target. British Journal of Dermatology, 171, 446-449.
tion of transcription factor AP-1 in human skin fibroblasts.
Journal of Investigative Dermatology, 130(6), 1697-1706.

Formulating | C&T ®
KEY POINTS
• One cosmetic strategy adopted to protect skin
against environmental pollution is the inclusion
of antioxidants in topical formulations.
• The present column reviews the synthesis

and extraction of vitamin E, and its structure
and utility for these applications.
INGREDIENT PROFILE
Vitamin E
E
Defeating Free Radicals
Prashant Bahadur and

Saroja Narasimhan, Ph.D. nvironmental pollution around the world
Johnson & Johnson has sparked significant growth in the rising
Skillman, NJ segment of skin care and cosmetic products
for anti-pollution protection. In many Asian
cities, for example, extreme pollution is a
part of life. This has increased consumer
awareness and concern regarding environmental pollutants on skin.1
One cosmetic strategy adopted to protect human skin against
environmental pollution is the inclusion of antioxidants in such

CT1903_Formulating_JJ_fcx.indd 42 4/17/19 9:31 AM

Besides antioxidant and moisturizing
The primary role of properties, studies have demonstrated that
vitamin E acts topically to protect against UVB
vitamin E in skin damage.10, 11 Topically applied a-tocopherol has
been shown to inhibit UVB-induced edema and
is to prevent erythema, conferring an SPF of 3 after multiple
applications.12 This benefit is attributed to
damage induced by the ingredient’s apparent ability to marginally
absorb light while functioning as a free-radical
reactive oxygen quenching, lipid-soluble antioxidant.12-14
Esters of vitamin E spread onto the skin
species. very easily and are rapidly absorbed, impart-
ing pleasant sensory attributes. The skin is left
shiny, elastic and non-greasy. Also, as it is not
a foreign molecule to the skin, the ingredient
formulations.2-4 The most common types of anti- rapidly integrates with the lipids in the skin.13
pollution ingredients are antioxidants, which After topical application, vitamin E supports
help to reduce the formation of oxygen free the extracellular lipid matrix of the stratum
radicals that can damage skin and accelerate corneum, to which vitamin E contributes its
the aging process.5 Anti-pollution products are antioxidant defenses.
broadly classified based on their mechanism of Interestingly, products containing both
action; they are also a new driver for multifunc- vitamins C and E have shown greater photopro-
tional cosmetics incorporating combinations of tection efficacy than either antioxidant alone.
ingredients to provide protection from envi- These synergistic effects are due to vitamin C’s
ronmental stress, such as UV light, while also ability to regenerate oxidized vitamin E.15, 16
moisturizing skin.6
Ingredient Sourcing
Skin Benefits As one of the most common antioxidants
In skin, the primary role of vitamin E, also used in cosmetic products, vitamin E is a
known as a-tocopherol, is to prevent damage generic descriptor for any form of tocopherol
induced by reactive oxygen species. These free or tocotrienol that acts as a vitamin with
radicals are actors in many skin problems; i.e., antioxidant properties.5, 10, 17, 18 Tocopherol is
sunburn, skin photoaging and hyperpigmenta- found largely in plant materials; it is also found
tion. Vitamin E has the potential to mitigate in vegetable fats and oils, dairy products, meat,
these effects, as it can scavenge free radicals eggs, cereals and nuts. Natural sources of
including hydroxyl, singlet oxygen and super- tocopherols include sunflower, peanut, walnut,
oxides Due to these antioxidant properties, the sesame and olive oils. Tocopherols and their
ingredient is used in a variety of cosmetic and esters are synthesized by chemical reactions
personal care formulations, such as creams, as well as vegetable oil distillation. Used as a
lotions, balms and other topically applied prefix, d (i.e., d-a-tocopherol) indicates a natural
formulations. The recommended use level source, while a dl prefix (i.e., dl-a-tocopherol)
is application-dependent, and ranges from indicates synthesis from a chemical reaction.9
0.5-5.0%.
Popular claims for vitamin E include:8, 9
• Anti-inflammatory agent
• Antioxidant
• Biodegradable ingredient
The global vitamin E market is expected to
• Promotes healing
attain a CAGR of 5.2% from 2018 to 2023, due
• Moisturizing agent to its rising application scope particularly in the
• Natural product treatment of lifestyle diseases.
• Plant-derived/vegetal-based
• Skin protection
Source: ResearchandMarkets

Vitamin E
Tocopherols and tocotrienols are amphiphilic nation of stereochemistry and double bond
lipids that share a substituted chromanol core; geometries, or mixtures thereof.
together, they comprise vitamin E. The two dif- In addition, vitamin E is comprised of eight
fer structurally by the substitution on the polar naturally occurring structural analogs: four
chromanol core by either: a lipophilic, saturated tocopherols (a-, b-, g- and d-analogs) and four
phytyl side chain; or by an unsaturated, isopren- tocotrienols (a-, b-, g- and d-analogs), deter-
oid (geranylgeranyl) side chain.3 Synthetically mined by the number and position of methyl
produced tocopherols are commonly racemic groups on the chromanol ring19 (see Figure 1
mixtures, whereas the synthetically produced for the chemical structure of each form).
tocotrienols can potentially have any combi- Tocopherol is readily oxidized upon expo-
sure to atmospheric
conditions or light, but
the oxidation propen-
sity varies among a-,
b-, g- and d-analogs,
due to differences in
oxidation potential
and reactivity with
molecular oxygen.9
Most topical tocoph-
erol preparations are
available in ester form,
such as tocopherol
acetate, since tocoph-
erol presents stability
concerns.20, 21 Addi-
Figure 1. Vitamin E forms tional esters include

tocopherol linoleate,
tocopherol nicotinate,

tocopherol succinate, etc. Conversion to tocoph- As an alternative, supercritical fluid extrac-
erol, the more bioactive form, is required for tion (SFE) uses gas as the solvent and operates
targeted action; the rate of hydrolysis for the ester at its critical point. Carbon dioxide is usually
is the rate-limiting step for the bioactivity of the used for this method. SFE to derive vitamin
vitamin E. E has been carried out with materials such as
a-Tocopherol and its esters are fat-soluble soybean oil deodorizer distillate, rapeseed oil
and colorless to pale-yellow, viscous oils. Both deodorizer distillate, sunflower oil deodorizer
are readily soluble in ethanol, chloroform and and palm oil.22
acetone but insoluble in water. They are typically Molecular distillation is another way to
stored at temperatures of 15-25°C under inert gas, extract vitamin E and reduce the toxicity
as they are sensitive to air and light.19 concerns associated with solvent extraction.
Synthesis of tocopherols and their esters Molecular distillation is a separation process
utilizes a Friedel-Crafts-type condensation of based on differences in molecular weights and
2,3,5-trimethylhydroquinone with synthetic performed under vacuum. It can be carried out
isophytol in an inert solvent (i.e., benzene or at very low temperatures, which reduces the
hexane) with an acid catalyst (i.e., zinc chloride, potential for damaging the extracted material.22
boron trifluoride or orthoboric acid/oxalic acid)
to create a-tocopherol (see Figure 2).5 Tocoph-
eryl acetate, linoleate/oleate and nicotinate are
prepared by the esterification of tocopherol with
the respective acid.
Claims for vitamin E
Tocopherols and other natural forms of
vitamin E also can also be extracted from the
include: antioxidant,
products and by-products of crude palm oil refin-
ing (see Figure 3).22 This extraction is carried
healing, skin
out in several ways. Solvent-based extraction protectant,
is widely utilized, and organic liquids such as
short chain alcohols are the most commonly anti-inflammatory
used solvents. However, due to the demand for
high purity and low costs, solvents that have and natural.
less of an impact on health and the environment
are preferred.

Vitamin E
Tocopherol prepared syntheti-

cally requires mixing the eight
stereoisomers; therefore, extrac-
tion of natural vitamin E is still
preferred. In its natural extracted
state, vitamin E is already
mixture of several tocopherol iso-
mers, which can help to stabilize
the more valuable d-a-tocopherol
isomer. Natural d-a-tocopherol
is moderately stable on its own,
and is thus often supplied as a
powdered acetate or succinate
complex.23 Natural vitamin E
acetate is formed by the esterifica-
tion of natural d-a-tocopherol
with acetic acid, a process that
is used to replace the unstable
hydroxyl group with an acetate
ester group.
Conclusion
With growing consumer inter-
est in anti-pollution products,
alongside the multifunctional
benefits of vitamin E—not to
Figure 2. Tocopherol synthesis mention its natural status—this
long-standing cosmetic ingredient
will no doubt continue to with-
stand the test of time.
References
1. Mistry, N. (2017). Guidelines for formulat-
Crude Palm ing anti-pollution products. Cosmetics,
4(4) 57.
Oil from
2. Juliano, C., and Magrini, G. A. (2018).
Fresh Fruit Cosmetic functional ingredients from
Bunches botanical sources for anti-pollution skin
care products. Cosmetics 5(1) 19.
3. Sakamoto, K., Lochhead, R., Maibach,
H., and Yamashita, Y. (2017). Cosmetic
By-products
Science and Technology: Theoretical
Refining or Principles and Applications, Elsevier.
Fractionation
4. Velasco, M. V. R., et al. (2018). Active
ingredients, mechanisms of action and
efficacy tests of antipollution cosmetic
and personal care products. Brazilian J
Pharma Sci 54.
5. Dreher, F., and Maibach, H. (2001).
Fatty Acids Deodorized Palm Olein Palm Stearin Biodiesel Protective effects of topical antioxidants
Palm Oil in humans. Current Problems in Derm
29 157-64.
6. Mausner, J. (1996). U.S. Patent No.
5571503. Assigned to Chanel Inc.
7. Lobo, V., Patil, A., Phatak, A., and
Figure 3. Vitamin E sourcing Chandra, N. (2010). Free radicals, anti-
oxidants and functional foods: Impact
on human health. Pharmacogn Rev 4(8)
118-126.

8. Hallstar (accessed 2019, Feb 25). Biochemica vitamin E 16. Traber, M. G., and Stevens, J. F. (2011, Sep 1). Vitamins C
natural product sheet. Retrieved from https://www.hallstar. and E: Beneficial effects from a mechanistic perspective,
com/product/vitamin-e-naturaltm/ Free Rad Bio and Med 51(5) 1000–1013.
9. Cosmetic Ingredient Review (accessed 2019, Feb 25). 17. Thiele, J. J., Schroeter, C., Hsieh, S. N., Podda, M., and
Safety assessment of tocopherols and tocotrienol as used in Packer, L. (2001). The antioxidant network of the stratum
cosmetics. Retrieved from https://www.cir-safety.org/sites/ corneum. Current Problems in Derm 29 26-42
default/files/tocoph032014FR.pdf 18. Traber, M. G., and Sies, H. (1996). Vitamin E in humans:
10. Maalouf, S., El-Sabban, M., Darwiche, N., and Gali-Muhtasib Demand and delivery. Annu Rev Nutr 16 321-347.
H. (2002). Protective effect of vitamin E on ultraviolet B light- 19. Robert, C. (2000). Vitamin E. In Kirk-Othmer, ed., Encyclope-
induced damage in keratinocytes. Molecular Carcinogenesis dia of Chemical Technology. Hoboken, NJ U.S., John Wiley
34 121-30. and Sons.
11. Ramos-e-Silva, M., Celem, L. R., Ramos-e-Silva, S., and 20. Bissett, D. L. (2009). Common cosmeceuticals. Clinics in
Fucci-da-Costa, A. P. (2013). Anti-aging cosmetics: Facts Derm 27 435-445.
and controversies. Clinics in Derm 31 750-758.
21. Shapiro, S., and Saliou, C. (2001). Role of vitamins in skin
12. Draelos, Z. D. (2011). Cosmetics and Dermatological care. Nutrition 17(10) 839-844
Problems and Solutions. New York, Informa Healthcare.
22. Maarasyida, C., Muhamad I., and Supriyanto, E. (2014).
13. Manela-Azulay, M., and Bagatin, E. (2009). Cosmeceuticals Potential source and extraction of vitamin E from palm-
vitamins. Clinics in Derm 27 469-474. based oils: A review. J Teknologi 69 4.
14. Draelos, Z. D. (2018). Updates in medical skin care. 23. Howard, J. (accessed 2019, Feb 25). Parchem is the
Advances in Cos Surg 1 211-217. premier supplier of vitamin E. Retrieved from https://www.
15. Burke, K.E. (2007). Interaction of vitamins C and E as better parchem.com/news-articles/Parchem-is-the-Premier-
cosmeceuticals, Derm Therapy 20 314-21. Supplier-of-Vitamin-E-N000152.aspx

KEY POINTS
• Dry masks are based on three technologies
that have revolutionized the cosmetic
industry: cosmetotextiles, delivery systems
and sheet masks.
• The described work sought to overcome

the limitations of these technologies,
resulting in a dry mask format. Its efficacy
is tested here.
DIRECTConnect Dry Mask Vectors Drive Active Delivery

Blandine Mosna, Joannie Emond, Katia Trudeau,
D
Marie-Ève Leclaire, Pierre Simard, Ph.D., Geneviève Nault,
Marie-Hélène Dufresne, Ph.D., and Karine Théberge, D.V.M.
Biomod Concepts Inc., Quebec
Dry Mask Foundation

ry mask product Cosmetotextiles: A cosmetotextile is a textile
forms are article that contains a substance or a preparation that
based on three is intended to be released sustainably onto the different
fundamental superficial parts of the human body, especially
technologies that the skin, and which claims particular
have revolution- properties such as cleansing, perfum-
ized the cosmetic industry in the past 10 to ing, change of appearance,
15 years: cosmetotextiles, active ingredient protection, maintenance in good
delivery systems and sheet masks. Combining condition, or correction of
and optimizing these innovations allows for body odors, according to the
synergized benefits, and has emerged as a new French Bureau de Normalisa-
way to apply skin care products for enhanced tion des Industries Textiles et
efficacy (see Figure 1a-b). This article consid- de l’Habillement.1
ers what these technologies can lend to dry When introduced on the
mask innovation and how to optimize them; the market, this innovation not only
resulting dry masks were then put to the test provided functionality but also
in vitro and clinically. ensured that the preparation

48 | www.CosmeticsandToiletries.com
Reproduction in English or any other language of all or part of this article is all or part
strictly of this article
prohibited. © 2019is strictly
Alluredprohibited.
Business Media. Vol. 134, No. 5 | May 2019
CT1905_Formulating_Mosna_fcx.indd 48 4/17/19 9:53 AM


Direct Connect
a)
Traditional delivery
systems are
limited in terms of
the number and
solubility of the
b) actives they
can contain.
containing solid microcapsules was released

through the stretching of the textile itself and
friction against the skin. Albeit promising, this
technology quickly encountered a few limita-
tions—some studies revealed toxic potential
and allergic reactions due to the nature of the
microcapsule’s shell and the excessive and
irregular amount of substance left on the skin
after release.2
Active ingredient delivery: Numerous
delivery systems are currently available, such as
liposomes, polymeric particles and molecular
a) Pink pattern corresponds to agglomerates of complexes, to help active ingredients penetrate
microparticles; and the skin.3, 4 These systems vary in structure, size
b) Depiction of a model wearing the dry mask by
slipping it over her ears. Use instructions indicate and mechanism with which they interact with
gently massaging for a few seconds to trigger the skin.5 Although first considered for pharmaceu-
transfer of microparticles to the skin. Immediately after tical applications, these vectors were introduced
removal, the skin is soft, smooth and hydrated. The dry
mask can then be folded and returned to the package into cosmetics and they considerably improved
for future uses. product efficacy. They quickly became a major
innovation for the beauty industry.
Figure 1. Schematic representation Despite their unquestionable value for
of an anti-aging dry mask enhancing skin penetration, traditional delivery
systems are limited in terms of the number
and solubility of the actives they can contain.
For example, the contained actives must have
the same lipid- or water-solubility, and cocktails
of ingredients can rarely coexist within the
The global facial sheet mask market was same delivery system.
valued at $2.91 billion in 2017 and is projected Sheet masks: Sheet masks are a relative
to expand through 2023 at a CAGR of 8.7% to newcomer to the skin care industry. First
reach $4.8 billion. extremely popular in Asia, they have been
winning international popularity since 2015.
Sheet masks can be made of paper, fiber, cotton,
Source: ResearchandMarkets
cellulose, foils or coconut pulp sheets, and
are soaked in skin care liquid. The products

are packaged individually and are intended the skin’s composition, and are readily compat-
for single use only. Their appeal is based on ible with the skin. Fatty acids, triglycerides
the close contact they make with skin, reduc- and sterols are naturally present in skin, so by
ing water evaporation and enhancing active supplying these ingredients, the delivery system
ingredient penetration. However, since the could itself help to restore the skin barrier.
liquid has an important aqueous phase, this Furthermore, through careful optimization of
can potentially accelerate the degradation rate not only their composition but also the prepara-
of unstable ingredients6 or, in some cases, the tion process, the particles also can incorporate
growth of bacteria. actives of different origins, physicochemical
properties and solubilities. Figure 2a-b shows
Dry Mask Development the colocalization of coumarin-6 and rhoda-
As noted, the development of dry masks mine B fluorophores, as markers for lipophilic
originated from the potential of these different
technologies and trends. The key objective of
the described work was therefore to look for
ways to overcome their inherent limitations, for
more efficient and innovative product develop-
ment and to answer the growing demand for
masks; especially sheet masks. In fact, Data-
monitor estimates the mask market value will
reach €6.6 billion (US $7.47 billion) by 2020,
with a CAGR of 8.1% between 2015–2020. It
also has been projected that in 20 years, 80% of
textiles will be technically adapted or function-
alized in some manner.1
Nonwoven dry masks can be considered a
close cousin to cosmetotextiles because they
incorporate ingredients into a textile form.
The present invention, however, also leverages
two patented technologies: a skin-mimicking
microparticle delivery system, and a patented,
dry-touch application process. Figure 3. Schematic representation
Microparticles: The microparticles are of dry mask applied to skin
composed of lipid-based ingredients to mimic
Panel C corresponds to superimposed images a and b; coumarin-6 has a log Po/w of 4.78 (lipophilic model); rhodamine B has a
log Po/w of 1.78 (hydrophilic model)
Figure 2. Confocal microscopy images of loaded microparticle under green channel

(lex = 488 nm) (a) and red channel (lex = 543 nm)(b)

Direct Connect
Materials and Methods

The transfer of Encapsulation: Microparticles contain-
microparticles ing the fluorescent markers rhodamine B
(0.02% w/w) and coumarin-6 (0.005% w/w)
to the skin is were first prepared as described previously.7
These particles were washed three times
modulated by with buffer and collected by centrifugation
(13,000 rpm). Localization of the loaded
parameters such as active ingredients within the micropar-
ticles was observed using a laser scanning
textile stretch, confocal microscopea.
Active payloads: Several ingredients were
body heat, incorporated into different sets of micropar-
ticles to test for various capacities, as described
movement and below. For transport to skin in general, a
liposoluble red dye was incorporated; to assess
massage. the effects of friction on transport, caffeine was
utilized; and to determine the penetration of
actives into skin, caffeine and/or niacinamide
and hydrophilic active ingredients, coincorpo- were included.
rated in the particles. In the context of anti-aging benefits, several
Thus, the particles primarily fulfill two agents were loaded simultaneously into the
topical application objectives: to modulate or microparticles at their recommended doses,
assist the barrier function of the skin, and to not only for multiple benefits, but also to assess
administer active ingredient(s) to one or more the behavior of multiple molecules. Test actives
skin layers or compartments. included: tetrapeptide-30b, to improve the
Dry-touch application process: The dry evenness and brightness of skin tone; Spilanthes
masks are obtained by applying the prepared acmella flower extractc, to stimulate fibroblasts
microparticles onto a textile via a patented and strengthen the collagen network; palmitoyl
process that results in a dry-to-the-touch isoleucined, for skin elasticity; Epilobium angus-
feel. This process enables the customization tifolium flower/leaf/stem extracte, to scavenge
of shape, pattern, color and formulation for free radicals; plankton extractf, for collagen
various cosmetic and, potentially, pharmaceuti- synthesis; and tocopheryl acetateg as an added
cal applications. Figure 1a depicts one such antioxidant. Finally, the loaded microparticles
dry mask featuring a pink formula applied in a were deposited onto nonwoven neck and
scallop pattern. facial masks using the proprietary dry-touch
When the mask is worn, the micropar- transfer process.
ticles are gradually transferred to the skin Transfer to the skin: To assess microparticle
by parameters such as textile stretch, body transport to skin, neck masks were applied for
heat, movement and massage (see Figure 3 15 min to healthy women volunteers over the
schematic). Upon contact with the skin, age of 30. Pigmentation from the liposoluble
the microparticles are destabilized by body red dye in the microparticle masks was mea-
temperature and friction while at the same sured before and after applicationh based on the
time their lipid matrix merges with the skin’s, a* parameter of the L*a*b scale (green to red
releasing the payload of active ingredients. Dry spectrum). Transfer was confirmed when the
masks do not require water, they are used as is,
in anhydrous form. a
Zeiss LSM 510 META, with inverted microscope
In the context of an anti-aging cosmetic, the b
Evonik
present article evaluates how a combination of c
Gattefossé
the microparticles with active payloads in the
d
SEPPIC
e
IFF Cosmetics
waterless textile mask could enhance active f
Barnet
ingredient penetration and, therefore, finished g
BASF
product efficacy. h
SkinEvidence system, Intuiskin

skin took on the red dye; in addition, the extent biopsy specimen was chosen to ensure the
of this transfer was indicated as a relative quantification limit of HPLC was reached.
increase in color on skin over time. The transfer Microparticle penetration: In vitro penetra-
of microparticles to skin was also measured tion studies were performed using Franz cells
by weight differences before and after the face in which membranesm were mounted between
masks were applied. donor and receptor compartments, per Haq.9
Effects of friction: Dry masks including The temperature at the surface of the synthetic
microparticles with caffeinej (5% w/w) were membranes was maintained at 32 ± 1°C.
applied to human skin biopsy specimens at a Microparticles loaded with actives containing
dose of 125 μg/cm2. Friction was then applied either 1.75% or 5.00% w/w caffeinen, and 1%
to the textiles using two methods, i.e., rotary or 2% w/w niacinamidep were prepared as
motion at various speeds, validatedk to mimic described previously.7
in vivo gestures and body movements.8 The Standard emulsions with caffeine and
masks were kept in contact with the biopsy niacinamide also were prepared using conven-
specimens for 8 hr, after which caffeine was tional and limited raw materials. In addition,
extracted from the textiles and quantified by commercial creams and serums containing
HPLC-UV. The amount of caffeine transferred caffeine or niacinamide were purchased at a
to the skin was obtained by the difference in local pharmacy. These standard emulsions and
applied dose; nine biopsies were used per test commercial products were used as controls for
condition. Note this long contact with the
m
Strat-M membranes, Millipore Sigma
j
Sigma-Aldrich n
Sigma-Aldrich
k
Eurofins ADME Bioanalysis p
Medisca

Direct Connect
comparison with the microparticle-loaded dry at baseline, 3 hr, 4 days (i.e., 24 hr after the
masks and contained the same percentage of third application) and 7 days (i.e., 24 hr after
active molecules. the sixth application) post-treatment using a
A fixed amount of formula (100 mg) was 3D skin measuring devices and corneometert,
placed onto the skin-like membranes for all respectively. During the clinical studies, no sign
test samples. For the control solutions, 500 µL of either cutaneous irritation or intolerance was
were deposited on the membranesm to perform observed (data not shown). Moreover, before
the assays. A phosphate-buffered saline solu- clinical studies, in vitro ocular assays and patch
tion (0.01 M, pH 7.4) was used as the receiver tests were performed to demonstrate innocuity
medium. The diffusion studies were stopped of the product.
after 420 min of contact time.
The amount of caffeine and niacinamide Results and Discussion
recovered from the receiver medium was quan- Transfer to skin: When the dry masks con-
tified at predetermined time points: 120 min, tacted skin, the microparticles detached from
240 min and 420 min. The caffeine and niacina- the textile sheet and gradually delivered their
mide content was assayed by HPLCq. Caffeine contents. This transfer was demonstrated using
and niacinamide detection was carried out by the red tracer dye, which left a measurable red
UV at 275 nm and 220 nm, respectively;10 all tint on the skin (see Figure 4a). Furthermore,
solventsr used were HPLC grade. after continued or subsequent contact, the
Clinical anti-aging studies: Dry masks with relative color change, i.e., transference, could
the anti-aging microparticle blend were applied be quantified over time (see Figure 4b). Both
for 15 min daily to the faces of 15 Caucasian measurements not only confirmed the trans-
women, 37-65 yrs old; 58 ± 2. The cutaneous fer of microparticles to the skin in as few as
relief parameters of the crow’s feet area— 15 min, but also highlighted the reusability of
i.e., average roughness (Ra), average relief the dry masks; the same amount of micropar-
(Rz) and maximum relief amplitude (Rt)—and ticles was transferred to the skin after a second
the cutaneous hydration rate were evaluated or third application.
q
Agilent 1220 Infinity LC equipped with Poroshell 120 EC-C18 s
3D Primos Lite (GFM)
column (2.7 μm, 4.6 x 100 mm) t
Corneometer CM 825, Courage + Khazaka
r
Fisher Scientific
a) b)
N = 5; mean ± SD, * = p < 0.05 compared with basal skin color
Figure 4. Transfer of microparticles to skin and change in skin redness, a*, after application
for 15 min (a) and reapplication of the same mask for 15 min on two subsequent days (b)

Effects of friction: This transfer of from targeting the deeper layers of the skin.
microparticles to the skin is modulated by Compared with commercially available formu-
parameters such as textile stretch, body heat, lations, the microparticle system accelerated
movement and massage. This was demon- their passage through the skin-like membranesm
strated ex vivo on human skin biopsy specimens at all time points and allowed greater amounts
(see Figure 5). Here, the amount of caffeine
transferred to the skin from the dry mask
increased by 2.5 and 10 times when two differ-
ent friction methods were applied as external
stimuli, demonstrating how body movement
and massage improve the efficiency of mic-
roparticle transfer to the skin.
Microparticle penetration: Once trans-
ferred to the skin, the microparticles fulfilled
their role as delivery vectors and enhanced the
penetration of the loaded active ingredients.
The percutaneous absorption experiments
with both caffeine and niacinamide demon-
strated this. Caffeine is a widely researched
molecule11 that acts on adipocytes located in
the hypodermis. Niacinamide, however, is a
water-soluble vitamin often used in commercial
N = 9, mean ± SD
beauty products as a whitening agent, with
reported benefits to repair and protect against
UV-induced skin damage, reduce wrinkles and
Figure 5. Demonstration of body movement and
massage factors influencing the transfer of caffeine
make the skin look healthier.12
As described, both molecules were used via microparticles
as model active ingredients that could benefit
a) b)
(a) Caffeine-loaded microparticles versus a commercial cream, standard emulsion and caffeine solution; diffusion at 420 min = 1.5× that of
commercial products
(b) Niacinamide-loaded microparticles versus a commercial cream, standard emulsion, commervial serum and niacinamide solution; diffusion at
420 min = 6× that of commercial cream; kinetics of niacinamide diffusion demonstrated identical values for both doses (1% w/w and 2% w/w)
incorporated in the microparticles
N = 3–6, mean ± SD, * = p < 0.05
Figure 6. Diffusion comparisons of caffeine (a) and niacinamide (b)

Direct Connect
a) b)
(a) Average roughness (Ra), average relief (Rz) and maximum relief amplitude (Rt)
(b) Parameters were measured at baseline, 3 hr, 4 days and 7 days
N = 15, mean ± SEM, p < 0.05 for all parameters, compared with baseline
Figure 7. Clinical efficacy of dry masks in terms of cutaneous relief

parameters (a) and hydration (b)
of both caffeine and niacinamide to be recov- skin smoothing (Ra), wrinkle reduction (Rz
ered in the receiver medium, indicating greater and Rt) and hydration benefits were observed
bioavailability (see Figure 6a-b). 3 hr hours post-application of the anti-aging
The microparticle-embedded dry mask dry mask.
proved even more advantageous than a com- The anti-wrinkle and hydration benefits
mercial serum, speeding up permeation time improved with time, confirming the cumulative
almost twofold—given that it took more than benefits of multiple applications of the mask
400 min to reach the niacinamide concentra- (see Figure 7, D4 and D7). It was hypothesized
tion already reached at 210 min using the that due to the biomimetic composition of the
microparticle technology (see Figure 6b). microparticles, the dry masks helped to restore
Clinical anti-aging effects: Having con- the skin barrier and recover its functionality
firmed the transfer of microparticles to the with each application.
skin and their improved skin penetration,
clinical studies aimed to demonstrate the Conclusion
clinical efficacy of an anti-aging dry mask. As Dry masks are nonwoven, textile-like sheet
noted, the dry masks contained a blend of both masks that can deliver active ingredients to
water-soluble and oil-soluble active ingredients the skin safely and effectively without the need
to fight free radicals, lift and smooth the skin, for water. By incorporating actives loaded into
correct and fill wrinkles, and brighten skin as the specialized microparticle delivery system
well as reduce the appearance of age spots. described, and using a patented dry touch
Women with dry facial skin and wrinkles application process, the present work shows
and fine lines in the crow’s feet area applied how an anti-aging dry mask enhanced the skin
anti-aging dry masks for 15 min on six consecu- penetration of loaded actives, contributing to
tive days. As shown in Figure 7a-b, immediate demonstrated finished product efficacy.

Thus, leveraging concepts from cosmeto- mask for topical delivery. AAPS Pharm Sci Tech, 11(3),
textiles, drug vectorization and sheet mask 1164-1170.
technologies, dry masks are pushing the market 7. Theberge, K., Goudreault, I., Quirion, F., and Perron, G.
(2018, Jan. 9). Article of manufacture releasing an active
boundaries as a convenient, easy-to-use and
ingredient. US Pat 9,861,154B2, assigned to Biomod Col-
effective new product category. lection Inc.
8. Dufresne, M. H., Hadjeb, D., Simard, P., Theberge, K.,
Leblond, A., Duchene, P., and Gelis, C. (2014). Dermal
References
transfer of active ingredients from Dermotex printed textiles:
1. Upadhayay, H., Jahan, S., and Upreti, M. (2016). Cosmeto- Development of an innovative in vitro model. Perspectives
textiles: Emerging trend in technical textiles. IORS JPTE 3(6) in Percutaneous Penetration, 14th International Conference.
8-14. La Grande Motte, France.
2. Tiwari, D., Upmanyu, N., Malik, J., and Shukla, S. (2017). 9. Haq, A., Dorrani, M., Goodyear, B., Joshi, V., and Michniak-
Cosmetotextiles used as a medicine. IJAPCR, 3(4), Kohn, B. (2018). Membrane properties for permeability
814-828. testing: Skin versus synthetic membranes. Int J Pharm,
3. Egbaria, K., and Weiner, N. (1990). Liposomes as a topical 539(1-2), 58-64.
drug delivery system. Adv Drug Deliver Rev, 5, 287-300. 10. Usher, K. M., Simmons, C. R., Keating, D. W., and Rossi,
4. Müller, R. H., Radtke M., and Wissing, S.A. (2002). Solid H. F. (2015). Determination of niacinamide in lotions and
lipid nanoparticles (SLN) and nanostructured lipid carriers creams using liquid-liquid extraction and high-performance
(NLC) in cosmetic and dermatological preparations. Adv liquid chromatography. J Chem Educ, 92(5), 907-910.
Drug Deliver Rev, 54, S131-S155. 11. Luo, L., and Lane, M. (2015). Topical and transdermal
5. Patravale, V. B., and Mandawgade, S. D. (2008). Novel delivery of caffeine. Int J Pharm, 490(1-2), 155-164.
cosmetic delivery systems: An application update. Int J 12. Wohlrab, J., and Kreft, D. (2014). Niacinamide—Mecha-
Cosmetic Sci, 30, 19-33. nisms of action and its topical use in dermatology. Skin
6. Fathi-Azarbayjani, A., Qun, L., Chan, Y. W., and Chan, S. Pharmacol Physiol, 27, 311-315.
Y. (2010). Novel vitamin and gold-loaded nanofiber facial
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KEY POINTS
• This study explores two formula parameters
that could potentially influence the diffusion
of an active through a hydrogel: the gelling
agent and the preservative system.
• Here, caffeine was used as the active,

along with a range of 12 gelling agents in
a simple hydrogel formulation, with and
without preservatives.
Rachael Polowyj, Milica Stevic and
Slobodanka Tamburic, Ph.D.
ActiveTransport
London College of Fashion, London, UK
How Rheology Modifiers and Preservatives Impact Release
I
Editor’s note: The following paper was first presented
in 2018 as a poster at the IFSCC Congress in Munich.
t is known that diffusion and through this structure before To start this process, however,
partitioning are the two most partitioning into the dermis, if the active ingredient must be
important phenomena in applicable. These processes are released in the first place; i.e.,
the complex process of skin dependent on the properties of it has to diffuse through the
penetration.1 A diffusing per- both the active ingredient and formulation and reach the SC in
meant must undergo a series the topical formulation used for sufficient quantity. For the given
of consecutive steps to penetrate its delivery. active, the diffusion is known to
the skin. First, the molecule must Generally, a topical active be dependent on the structural
diffuse through the formulation should have the following char- properties of the 3D network of
to the skin surface and partition acteristics in order to penetrate the vehicle.
into the skin, before diffusing skin efficiently: an octanol-water For the present study, caf-
through the stratum corneum (SC) partition coefficient of about 100 feine served as the model for
via one of the three delivery routes: (Log Po/w = 2); good solubility in a hydrophilic cosmetic active.
intercellular, intracellular or via both lipophilic and hydrophilic It is a methylxanthine deriva-
skin appendages. media; and a relatively small tive with molecular weight of
It must then partition into molecular weight (MW);2 usually 194.2 Da and Log Po/w of -0.07.
the viable epidermis and diffuse belowReproduction
500 Da.in 3
English or any other language of Caffeine is increasingly used as
CT1905_Formulating_Polowyj_fcx.indd 58 4/17/19 10:42 AM

Reproduction in English or any other language of all or part of this article is strictly prohibited. © 2019 Allured Business Media. Cosmetics & Toiletries® | 59

Active Transport
Caffeine recovery generally increased

in the presence of preservative, with
small exceptions in the cases of sodium
carboxymethylcellulose and carrageenan.
a hydrophilic model substance for topical in Gelling agents: To form the hydrogel vehicle
vitro testing, due to its ability to penetrate the for the topical delivery of caffeine, 12 gelling
skin barrier4 and the ability to exert cosmetic agents (see Table 1) belonging to five chemical
effects; e.g., anti-cellulite and the reduction of categories were used, including:
periorbital puffiness. There is also evidence • Cellulose derivatives: sodium carboxymethyl
that caffeine possesses antioxidant properties, cellulose and hydroxyethyl cellulose;
which may protect cells against the effects of • Clays: hectorite and magnesium
UV radiation.5, 6 aluminium silicate;
Two formulation parameters that could • Natural polymers: xanthan gum, carra-
influence the diffusion of a hydrophilic ingredi- geenan and gellan gum;
ent, i.e., caffeine, through a hydrogel system • Polyacrylic acid polymers: carbomer,
were explored in this study: a gelling agent and acrylates C10-30/alkyl acrylate crosspolymer
a preservative system. The aim was to assess and sodium polyacrylate; and
whether, and to what extent, changes in rheolog- • Silica-based thickeners: hydrated silica
ical properties exerted by these two parameters and silica.
could affect the in vitro release of caffeine from
a hydrogel formulation. Sample preparation: The preparation of
samples followed a generic process, consisting
Materials and Methods of: dissolution of caffeine in water at 45°C with
stirring; dispersion and mixing of the gelling
A simple hydrogel formulation was devel-
agent; and addition of the preservative and/or
oped (see Formula 1). Given the fact that
pH adjuster, when required. This method was
gelling agents can have very different gelling
modified when the gelling agent had specific
potential, different concentrations were used,
requirements in terms of a higher temperature
sufficient to achieve a similar value of apparent
or the pH of the water used for dispersion.
viscosity. The target viscosity and pH, estab-
Rheology measurements: Rheological
lished by measuringa a suitable commercial
measurements (see Table 1) were carried with
benchmark, were 44,000 mPa.s at 20°C and a
a rheometerb using a 35-mm serrated parallel
pH of 5.93, respectively. A tolerance limit of
plate and the gap of 1 mm. Continuous flow
±20% from the above values was applied.
and dynamic (oscillation) tests were used in
a
Brookfield DV-E, Brookfield Ametek, UK, measured at 6 rpm with conjunction, to produce complete rheologi-
T-bar S93 and a helipath cal profiles of the test samples. Two types of
flow measurements were employed: the shear
rate sweep, from 250 sec-1 to 10 sec-1 during a
The global active ingredients market for period of 100 sec; and the three-step thixotropy
cosmetics was valued at $2.63 billion in method, at the constant shear rate of 10 sec-1,
2015 and is projected to reach $4.45 billion followed by 250 sec-1 and again, 10 sec-1, with
by 2026. each step taking 60 sec.
The oscillatory stress sweep was also
conducted to establish the viscoelastic proper-
Source: ReportBuyer
ties of the samples, and measured complex
b
RheoStress RS75 Rheometer, Haake

modulus G*, also known as rigidity, and the Testing was conducted over a 4-hr period and
phase angle d, or lag phase. This test was the sampling was carried out after 30, 60, 120,
carried out at the constant frequency of 1 Hz 180 and 240 min, followed by prompt replace-
and the oscillatory stress range of 0.5-500 Pa. ment of the receptor medium, i.e., phosphate
The method was also used to establish the yield buffered saline, pH 7.4, in order to maintain a
stress of each hydrogel, expressed as the stress constant volume in the cell.
values at which the complex modulus declines The concentration of caffeine was quanti-
by 10%. fied immediately after sampling using a
Caffeine release: Testing the in vitro release spectrophotometere at 275 nm and a standard
of caffeine was performed in a vertical diffusion curve for caffeine. Statistical analysis of the
cell test systemc consisting of 10 diffusion cells. release data was performed using repeated-
Experiments were carried out at a temperature measures one-way ANOVA, with p = 0.05 as the
of 32 ± 10°C and a stirring rate of 600 rpm, significance threshold.
through a hydrophilic membraned. The
membrane was composed of polysul-
fone and had a diameter of 25.0 mm, Formula 1. Generic Hydrogel Formulation
a pore size of 0.45 μm and a thickness
of 300 μm.
INCI Name % w/w
The release profile of caffeine for
Water (aqua) qs to 100.00
each hydrogel was determined by
Caffeine 2.00
taking 20-μL samples from each of 10
Gelling Agent qs to viscosity
diffusion cells and analyzing their caf-
Methylparaben 15% (and)
feine content spectrophotometrically . e
Ethylparaben 10% (and)
c
HDT 1000 vertical diffusion cell test system,
Phenoxyethanol 75% (if used) 1.00
Copley Scientific Citric Acid qs to pH
d
Tuffryn membrane, Pall Corporation, Sigma Aldrich Sodium Hydroxide qs to pH
e
NanoDrop 2000 UV-Vis Spectrophotometer,
Thermo Scientific
Table 1. Concentration, pH and Viscosity Values of Test Hydrogels
Viscosity without Viscosity with

Concentration pH without pH with
INCI Name preservative preservative
(% w/w) preservative preservative
(mPa.s) (mPa.s)
Sodium
3.75 6.60 6.95 45,500 45,700
Carboxymethylcellulose
Hydroxyethylcellulose 2.20 6.31 6.32 48,700 45,800
Xanthan Gum 6.00 7.08 6.69 40,000 42,700
Carrageenan 2.75 6.48 5.78 41,200 42,300
Gellan Gum 1.75 5.80 5.56 42,500 37,200
Hectorite 3.50 6.71 6.90 36,200 42,200
Magnesium Aluminium
2.50 6.69 6.49 41,200 40,000
Silicate
Carbomer 0.35 6.22 5.52 36,700 40,000
Acrylates/C10-30 Alkyl
0.35 6.02 6.23 50,200 44,300
Acrylate Crosspolymer
Sodium Polyacrylate 1.00 5.94 5.92 50,000 48,000
Hydrated Silica 13.50 6.29 6.23 50,200 38,700
Silica 6.00 5.33 5.94 41,300 52,800

Active Transport
Results and Discussion The sample with preservative showed

An example of one complete dataset obtained higher viscosity within the whole shear rate
for the gelling agent sodium carboxymethylcel- range, a finding that was mirrored in the
lulose is given in Figure 1a-d. These graphs three-step thixotropy test (see Figure 1b).
show results from the three rheological tests, This thixotropy test uses two shear rates,
shear rate sweep, thee-step thixotropy and in this case 10 sec-1 and 250 sec-1, to assess
oscillatory stress sweep, alongside the in vitro the effect of not only shear, but also of time
caffeine release profile for the samples with on the loss and subsequent recovery of the
and without the chosen preservative system. In sample structure, measured by the changes
common with all tested hydrogels, the sodium in viscosity.7 In addition to the graphs, the
carboxymethylcellulose sample showed a shear- method produces a quantitative measure in
thinning rheological behavior, with distinct yield the form of percentage of viscosity recovery
stress—i.e., the value of shear stress at which (see Table 2), calculated from the end parts
the material starts flowing; a behavior known as of the viscosity curves obtained in the first
plastic flow (see Figure 1a and Table 2). and third steps.
a) b)
c) d)
Using: shear rate sweep (a); three-step thixotropy test (b); and oscillatory stress sweep (c); plus, caffeine release profiles (d)
Figure 1. Rheological characterization of sodium carboxymethylcellulose hydrogel, with and

without preservative

All hydrogels released
100% of the caffeine
within four hours, with
the exception of
xanthan gum.
It is evident from Table 2 that the recovery The graph in Figure 1c shows the behavior
percentage generally increased in the presence of the two relevant parameters in this test: the
of preservative, with small exceptions in the complex modulus G* and the phase angle d.
cases of sodium carboxymethylcellulose and From this data it is clear the presence of the
carrageenan. The structure of the clay samples preservative strengthened the internal structure
could not withstand the high shear of the of the hydrogel, as evidenced by an increased
second step, hence no data was obtained for complex modulus G* and decreased phase
these hydrogels. angle d; the lower the phase angle, the higher
As a semisolid system, each hydrogel belongs the elasticity of the material.
to the group of viscoelastic materials, having Yield stress was detected as the point where
both liquid-like (viscous) and solid-like (elastic) the rigidity of the sample starts decreasing.
characteristics.8 Dynamic (oscillatory) rheology Since the yield stress is not a point but a region,
is a standard method used to assess viscoelastic- however, the same approach was used to detect
ity, whereby an oscillating shear stress is applied the yield value as previously published;7 i.e.,
to the sample and the resulting strain measured the value of stress causing the rigidity to fall
is its response.9 Dynamic tests are performed by 10% (see Table 2). It could be concluded
at very low shear stresses, normally below the from Table 2 that the addition of preserva-
yield point, to allow for insights into the internal tive considerably increased the yield value
structure of a semisolid without destroying it.10 for each hydrogel except in the case of the
The oscillatory stress sweep method, shown in three polyacrylic acid polymers, where it was
a recent study7 to be the most reliable for the almost unchanged.
detection of shear stress, was used to detect this Despite changes in the internal structure,
parameter in all samples. captured by rheological measurements, the

Active Transport
Table 2. Rheological Parameters via Three-step Thixotropy* and Oscillatory Stress Sweep** Tests
% Recovery without % Recovery with Yield stress without Yield stress with
INCI Name
preservative preservative preservative (Pa) preservative (Pa)
Sodium
93.86 87.13 19.62 69.26
Carboxymethylcellulose
Hydroxyethylcellulose 86.57 100.00 92.01 111.00
Xanthan Gum 88.79 91.83 83.66 101.70
Carrageenan 93.34 76.22 (-) 80.82
Gellan Gum 32.57 95.60 13.72 26.33
Hectorite (-) (-) 259.90 312.50
Magnesium Aluminium Silicate (-) (-) 135.10 200.00
Carbomer 95.56 96.55 34.87 28.02
Acrylates/C10-30 Alkyl
93.97 95.36 37.58 42.60
Acrylate Crosspolymer
Sodium Polyacrylate 92.37 98.26 85.11 83.18
Hydrated Silica 0.03 83.46 18.57 39.80
Silica 4.45 71.35 45.76 196.00
*percentage of structural recovery, measured by viscosity

** the value of yield stress
(-) in some cases, it was not possible to derive data under the conditions of the test
Table 3. In vitro Release of Caffeine from the Series of Hydrogels
% Released % Released % Released % Released

Significance Significance
after 30 min after after 4 hr after
INCI Name (p) after (p) after
without 30 min with without 4 hr with
30 min 4 hr
preservative preservative preservative preservative
Sodium Carboxymethyl
49.45 52.27 1.000 93.00 100.00 0.970
Cellulose
Hydroxyethyl Cellulose 63.70 16.63 0.000* 100.00 100.00 0.994
Xanthan Gum 14.99 9.03 1.000 83.19 66.69 0.996
Carrageenan 56.47 36.95 0.946 100.00 100.00 1.000
Gellan Gum 56.22 0.00 0.000* 100.00 100.00 1.000
Hectorite 34.08 51.51 0.984 58.09 98.18 0.039*
Magnesium Aluminium
23.93 42.30 1.000 50.23 100.00 0.001*
Silicate
Carbomer 47.90 70.64 0.807 99.90 53.13 0.004*
Acrylates/C10-30
Alkyl Acrylate 62.13 58.70 1.000 100.00 100.00 1.000
Crosspolymer
Sodium Polyacrylate 4.56 82.69 0.00* 85.29 100.00 0.571
Hydrated Silica 43.50 24.53 0.957 96.99 100.00 1.000
Silica 34.27 32.89 1.000 89.94 100.00 0.915
* significance at 5%

release profile of caffeine from the sodium detected during the first 3 hr with the tendency
carboxymethylcellulose sample stayed almost to equalize later (e.g., Figures 2a-c).
the same after the addition of preservative A deviation from the above observations
(see Figure 1d), with no significant changes was detected in the case of xanthan gum, which
observed at either 30 min or 4 hr (see Table 3). showed the lowest overall caffeine release. The
The overall release results, however, showed set of results for xanthan gum with and without
a variety of patterns. These were both gelling preservative is shown in Figure 3. Rheological
agent- and preservative-dependent. All hydro- results revealed little change in the internal
gels released 100% of the caffeine within the hydrogel structure, with almost identical
4-hr test, most of them between the first and viscosity, rigidity and elasticity (see Figures 3a
second hour with the exception of xanthan gum; and 3c) and a small increase in the percent-
it achieved a maximum release of 80% (see age of thixotropic recovery and yield stress
Table 3). The addition of preservative gener- (see Table 2). However, the in vitro caffeine
ally produced either identical or higher release release profile with preservative was consis-
rates than the samples without preservative tently, although not significantly, lower (see
(e.g., Figure 2d) but the difference was not Figure 3d). This indicates that the rheological
always significant. The exceptions were hydroxy- effect was not the only parameter affecting the
ethyl cellulose, hydrated silica and all of the diffusion coefficient of caffeine in xanthan gum.
natural gums, whereby a lower release rate was The fact that this hydrogel showed the lowest
a) b)
c) d)
Figure 2. Results of the in vitro release of caffeine from carrageenan (a), gellan gum (b),
hydrated silica (c) and silica (d) hydrogels

Active Transport
release rate for caffeine is congruent with an The hydrogel based on acrylates/C10-30 alkyl
earlier observation by Talukdar and Kinget.11 acrylate crosspolymer (see Figure 4) provides
They measured the diffusivity of three drugs, an example where the addition of preserva-
including caffeine, from the hydrated polymeric tive made small alterations to the internal
matrices of xanthan gum and hydroxypropyl structure. The viscosity, thixotropy level and
methyl cellulose and found that it was lower rigidity show small differences, while the phase
in the case of xanthan gum. They concluded angle d, expressing the sample’s elastic proper-
that the slow diffusion through the xanthan ties, was unaltered. In line with the theory, the
gum hydrogel was the controlling factor in the release profile of caffeine from the two varia-
retarded release of caffeine from the relevant tions of this formulation did not differ, either
tablets. This finding did not apply to the hydro- (see Figure 4d).
phobic actives tested in their experiments. Table 3 presents the results of the caffeine
In terms of the present study, it would be release from all the samples after 30 min and
useful to observe the release profile of caffeine 4 hr; statistical analyses were performed from
during a longer period (e.g., 8 hr) in order to a repeated measures one-way ANOVA test,
establish whether, and at which time point, a followed by Tukey HSD test. After 30 min, three
complete release of caffeine occurs. samples showed significant differences in caf-
a) b)
c) d)
Using shear rate sweep (a); three-step thixotropy test (b); and oscillatory stress sweep (c); plus, the caffeine release profiles (d)
Figure 3. Results of the rheological characterization of xanthan gum hydrogel, with and
without preservative

feine release; gellan gum is shown in Figure 2b.
After 4 hr, these differences in all three samples
were no longer apparent but new differences
emerged (see Table 3).
It should be noted that carbomer presented
an anomaly in terms of showing a decrease in
the percentage of caffeine released between
the first and fourth hour, which could be an
instrumental error. This leaves the two clays,
i.e., hectorite and magnesium aluminium
silicate, as the only hydrogels in which the
presence of preservative significantly increased
the release of caffeine after 4 hr. Since clays
have very specific, ion-dependent mechanisms
of gel formation, it is reasonable to assume the
diffusion of caffeine molecules was made easier
due to the rearrangement of platelets caused by
the presence of preservative.
Interestingly, the expected pattern of
decreased diffusion rate with increased viscosity
was not consistently observed. This revealed
the influence of additional factors affecting the
diffusion rate of caffeine through the hydrogel
system. It is known that diffusion through
polymeric networks takes place through the
liquid-filled pores, and that this mainly depends
on the pore size, tortuosity and partition coef-
ficient for the large pores.12 For the small pores,
however, it is also dependent on the
steric hindrance and sliding friction. It is
possible that some of these parameters were
changed by the addition of preservative but not
detected through rheological measurements,
and vice versa. Due to this complexity, it is not
possible to accurately predict the in vitro release
pattern of caffeine through the tested hydrogels,
apart from the fact that most of them release
100% of caffeine during the first 2 hr.
Conclusion
This study showed that the presence of
preservative, in addition to the type of gelling
agent, could strongly affect the rheological
properties of the hydrogel vehicles used for the
topical delivery of caffeine. For most hydrogels
evaluated in this study, the change in rheological
properties affected the rate of release of caffeine
from the formulation, hence this effect could
be used to control the initial stage in complex
topical delivery processes.

Active Transport
a) b)
c) d)
Using shear rate sweep (a), three-step thixotropy test (b), oscillatory stress sweep (c) and the caffeine release profiles (d)
Figure. 4. Results of the rheological characterisation of acrylates/C10-30 alkyl acrylate

crosspolymer hydrogel, with and without preservative
Acknowledgements: The authors wish to thank the London 7. Tamburic, S., Sisson, H., Cunningham, N., and Stevic, M.
College of Fashion for supporting this study and the Society C. (2017). Rheological and texture analysis methods for
of Cosmetic Scientists and Azelis UK, Ltd., for supporting the quantifying yield value and level of thixotropy. SÖFW, J
attendance of Rachael Polowyj at the IFSCC 2018 Congress. 143(6), 24-30.
8. Miner, P. E. (1993). Emulsions rheology: Creams and lotions,
in, Laba, D., ed. Rheological Properties of Cosmetics and
References Toiletries, New York, Marcel Dekker, 131-369.
1. Wiechers, J. W., et al. (2004). Formulating for efficacy. Intl J 9. Brummer, R. (2006). Rheology Essentials for Cosmetic and
Cos Sci, 26(4), 173-182. Food Emulsions. Hamburg, Springer.
2. Lane, M. E., et al. (2012). Rational formulation design. Intl J 10. Craig, D. Q., Tamburic, S., Buckton, G., and Newton, J. M.
Cos Sci, 34(6), 496-501. (1994). An investigation into the structure and properties
3. Bos, J. D., and Meinardi, M. M. H. M. (2000). The 500 of Carbomer 934 gels using dielectric spectroscopy and
Dalton rule for the skin penetration of chemical compounds oscillatory rheometry. J Control Rel, 30, 213-223.
and drugs. Exp Derm, 9(3), 165-169. 11. Talukdar, M. M. and Kinget, R. (1997). Comparative study
4. Luo, L., and Lane, M. E. (2015). Topical and transdermal on xanthan gum and hydroxypropylmethyl cellulose as
delivery of caffeine. Int J Pharm, 490, 155-164. matrices for controlled-release drug delivery. II. Drug diffu-
sion in hydrated matrices. Intl J Pharma, 151(1), 99-107.
5. León-Carmona, J. R., Galano, A. (2011). Is caffeine a good
scavenger of oxygenated free radicals? J Phys Chem, B 12. Karlsson, J., Stubbs, J. M., Karlsson, L. E., and Sundberg,
115, 4538-4546. D.C. (2001). Estimating diffusion coefficients for small mol-
ecules in polymers and polymer solutions. Polymer, 42(11),
6. Koo, S. W., Hirakawa, S., Fujii, S., Kawasumi, M., and 4915-4923.
Nghiem, P. (2007). Protection from photodamage by topical
application of caffeine after ultraviolet irradiation. Br J
Dermatol ,156, 957-964.

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Want More Formulas?

Click to Page DE1 of the May 2019 digital
edition for the expanded formulary, complete
with interactive links to the free
Cosmetics & Toiletries Bench Reference.
Anti-Aging Formulary
ANTI-AGING CREAM WITH C. Propanediol (and) Glycerin (and) Water (aqua) (and)
Asparagus Officinalis Stem Extract (and) Gluconolactone
PUERARIA MIRIFICA ROOT EXTRACT (and) Sodium Benzoate (and) Potassium Sorbate (and)
(Bio-Botanica Inc.) Calcium Gluconate (ReguScence, DSM Personal Care) 3.00
Fragrance (parfum) 0.30
A. Water (aqua) qs to 100.00% w/w
Procedure: Combine A in vessel with mixing. In separate vessel, sprinkle the
Phenoxyethanol 0.70
acrylates/C10-30 alkyl acrylate crosspolymer into the water of B with mixing,
Caprylyl Glycol 0.50 until uniform. Add remaining B with continued mixing. Add B to A with mixing.
Ceteareth-20 1.50 Homogenize @10,800 rpm for 1 min. Add C to batch with mixing. Homogenize
Lycium Barbarum (Goji) Fruit Extract (and) Coffea Arabica mixture agaom @8,000 rpm for 1 min.
(Coffee) Fruit Extract (and) Euterpe Oleracea Fruit Extract
(and) Morinda Citrifolia Fruit Extract (and) Punica Granatum
Extract (and) Garcinia Mangostana Fruit Extract (and)
Camellia Sinensis Leaf Extract (and) Propanediol
WRINKLE ERASER CREAM
(Superfruit Blend, Bio-Botanica Inc.) 2.00 (Grant Industries Inc.)
Cucumis Sativus (Cucumber) Fruit Extract (Cucumis A. Cyclopentasiloxane 8.00% w/w
sativus (Cucumber) Fruit Extract, Bio-Botanica Inc.) 2.00 Disiloxane 3.50
Mineral Oil 7.00 Isododecane (Creasil ID, The Innovation Company) 6.00
Stearic Acid 9.00 Polymethylsilsesquioxane (Gransil PSQ, Grant Industries Inc.) 4.00
Cetyl Alcohol 4.00 Phenoxyethanol (and) Ethylhexylglycerin (euxyl PE 9010,
Propylene Glycol 3.00 schulke) 0.50
Pueraria Mirifica Root Extract (Purestrol, Bio-Botanica Inc.) 3.00 B. Water (aqua) 30.60
Stearyl Alcohol 2.00 Carbomer (Carbopol Ultrez 10 Polymer, Lubrizol Advanced
Cetearyl Alcohol 2.00 Materials, Inc.) 0.20
Isopropyl Palmitate 0.25 Triethanolamine 0.20
B. Prunus Amygdalus Dulcis (Sweet Almond) Oil 0.30 Steareth-21 2.00
Glycol Monostearate SE 0.60 C. Polysilicone-11 (and) Water (aqua) (and) Laureth-12 (and)
Simmondsia Chinensis (Jojoba) Seed Oil 0.08 Phenoxyethanol (and) Ethylhexylglycerin (Gransil EP-9,
FD&C Yellow No. 6 0.20 Grant Industries Inc.) 45.00
Procedure: In main beaker, mix A under lightening mixer agitation and create a 100.00
vortex. Heat to 60°C. In a separate beaker, mix B to 60°C. Combine B into A
Procedure: Add A into main kettle and mix until uniform. Combine B in separate
and mix for 10 min or until fully dispersed at 60°C. Begin cooling under agitation.
kettle and heat to about 70°C with mixing until there are no lumps. Add B to A
When batch reaches 40°C, add C; properties: appearance = light, peach-colored
while mixing and mix until uniform. Add C to AB while mixing and continue to mix
cream; pH = 5.5-6.5.
until smooth and uniform.
YOUTH PRESERVING CARE

(Centerchem Inc.)
A. Simmondsia Chinensis (Jojoba) Seed Oil 2.00% w/w
Diethylhexyl Carbonate 6.00
Dimethicone 0.50
Tocopheryl Acetate 0.50
Acrylates/Acrylamide Copolymer 2.00
Squalane (Neossance Squalane, Amyris Inc.) 1.50
B. Water (aqua) qs to 100.00
Acrylates/C10-30 Alkyl Acrylate Crosspolymer 0.25
Glycerin 3.00
Preservatives qs
CT1905_Anti_Aging_Frmlry_fcx2.indd 70 4/19/19 11:05 AM

7ITH,UMI3ET 2ESINS,ONG ,ASTING.AIL#OATINGS.O,ONGER2EQUIRE56,AMPS

These all-new polyurethane resins use gel polish chemistries to add toughness and
durability to long-lasting nail polishes, without the usual obstacles. With LumiSet™
resins, there is:
• .O.EEDFOR56,AMPSThe resins air-dry tack free, and can be formulated

to cure with sunlight.
• .O.EEDFORAN!DDED"ASE#OAT The color coat materials offer excellent
adhesion to the nail bed, with no need for additional adhesion promoters.
• .O.EEDFOR0LASTICIZERSTheproducts are inherently flexible and tough,
with no need for additional plasticizers.
• .O.EEDFOR3OAKINGThe resins are easily removable with traditional
nail polish removers.
'ETHELPONYOURNEXTPROJECTTODAY \DYMAX OCCOMLUMISET

Advertiser Index | C&T ®
May 2019 | Volume 134, number 5
Beauty Accelerate Grant Industries MilliporeSigma

17 1 47
www.beautyaccelerate.com info@grantinc.com sigma-aldrich.com/flavors-fra-
www.grantinc.com grances
Bio-Botanica, Inc.
C2 RCTS, Inc.
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Campo Research Pte Ltd.
8
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www.campo-research.com Lipotec, LLC schülke, Inc.
7 5
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Centerchem, Inc.
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cosmetics@centerchem.com LipoTrue 35
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Contipro
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www.contipro.com Lucas Meyer Cosmetics 11
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Dymax Oligomers & Coatings
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Mibelle AG Biochemistry
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CT1905_Advertiser_Index_fcx.indd 72 4/17/19 11:00 AM

EXPANDED Anti-Aging Formulary
Continued from Page 70
LIFT ME GEL CREAM D. Polymethyl Methacrylate 2.00

E. Fragrance (parfum) 0.20
(The Hallstar Company) 98.00
Procedure: Heat A and B to 75-80°C. Add B in A under maximum stirring and main-
This soothing face cream is enriched with antioxidant
tain stirring rate for 3 min. Cool under medium stirring. Add C, D and E in order
Eurol BT and provides non-stop daily hydration to below 40°C. Adjust pH if necessary; formula specifications: aspect = off-white,
delay signs of aging caused by loss of moisture. Olivem bright cream; viscosity (Rheo ELV 8, spindle 4, 6 rpm, 3 min) = 100,000 mPa.s;
2020 refreshes and cools the skin on application. Oléos pH = 4.3-5.5; centrifugation (3,000 rpm, 20 min) = stable.
Lift Oléoactif reduces the appearance of fine lines and
improves skin density. A combination of Sensolene and
Biochemica Camellia Tea Oil provides deep hydration to AGE DEFENSE CREAM
support healthy skin elasticity. Oléos, based in France, is
a recently acquired part of Hallstar. (Mibelle Biochemistry)
A. Water (aqua) qs to 100.00% w/w A. Water (aqua) 61.00% w/w

Glycerin 3.00 Disodium EDTA 0.10
Betaine 0.40 Aminomethylpropanediol 3.00
Olea Europaea (Olive) Leaf Extract (and) Water (aqua) Ethoxydiglycol 2.00
(Eurol BT, The Hallstar Company) 0.25 B. Ceteth-20 (and) Cetyl Alcohol (and) Glyceryl Stearate (and)
Trisodium Ethylenediamine Disuccinate 0.30 Steareth-20 (Emulium Delta, Gattefossé SAS) 4.00
B. Camellia Oleifera Seed Oil (Biochemica Camellia Tea Oil, Benzyl Alcohol 0.50
The Hallstar Company) 2.50 Benzoic Acid 0.20
Ethylhexyl Olivate (Sensolene, The Hallstar Company) 2.00 Tocopheryl Acetate 0.20
Carthamus Tinctorius (Safflower) Seed Oil (and) Astragalus Hydroxyethyl Acrylate/Sodium Acryloyldimethyl Taurate
Membranaceus Root Extract (and) Ubiquinone (and) Copolymer 0.30
Tocopherol (and) Spilanthes Acmella Flower/Leaf/Stem Olea Europaea (Olive) Fruit Oil 1.00
Extract (Oléos Lift Oléoactif, The Hallstar Company) 1.00 Hydrogenated Vegetable Oil 1.00
Bisabolol 1.00 Stearyl Alcohol 0.80
Preservatives qs Myristyl Lactate 2.00
Lecithin (and) Tocopherol (and) Ascorbyl Palmitate (and) C10-18 Triglycerides 2.00
Citric Acid (Aperoxid TLA, Biochim Srl) 0.05 Hydrogenated Ethylhexyl Olivate 4.00
Ethylhexyl Olivate/Sodium Acrylates Copolymer/ Hydrogenated Olive Oil Unsaponifiables 4.00
Polyglyceryl-4 Olivate (Olivem 2020, The Hallstar Company) 2.00 Dimethicone 0.80
C. Cyclomethicone 8.00 C. Water (aqua) 10.00
Cyclopentasiloxane (and) Dimethiconol (Silsoft 1215 HV, Maltodextrin (and) Lecithin (and) Water (aqua) (and)
Momentive Performance Materials Inc.) 2.00 Coenochloris Signiensis Extract (Snow Algae Powder,
Dimethicone/Dimethicone/Vinyl Dimethicone Crosspolymer Mibelle Biochemistry) 3.00
(KSG-16, Shin-Etsu Silicones of America, Inc.) 1.00 D. Fragrance (parfum) 0.10
100.00
Procedure: Prepare A and B separately. Add A to B and homogenize using a suit-
able dispersion unit. Add C. Mix until smooth and uniform; properties (@25°C): Procedure: Mix A until dissolved and heat up to 70°C. Mix B and heat up to 70°C.
appearance = shiny white gel-cream; viscosity (10 rpm, Brk, RVDV-E, T-B, after At 70°C, combine A and B under strong agitation and homogenize. Cool under
24 hr at RT; mPa∙s) = 16,000–19,000; pH = 6.0–7.0. agitation. Combine C. Add C to batch below 40°C. Add D to batch. If necessary
adjust pH to 5.5-6.5 using E.
ANTI-PHOTOAGING ELIXIR
(Lucas Meyer Cosmetics)
Claims: • Light and cool texture • UV and IR protective

day cream • Paraben-free
A. Water (aqua) 70.70% w/w
Sodium Phytate 0.20
Glycerin 2.00
Glycerin (and) Picea Abies Extract (and) Alcohol (Granlux
AOX-GL, Oy Granula Ab Ltd.) 1.00
Phenoxyethanol 0.60
Chlorphenesin 0.30
B. Glyceryl Stearate Citrate (and) Polyglyceryl-3 Stearate (and)
Hydrogenated Lecithin (Heliofeel, Lucas Meyer Cosmetics) 4.00
Sodium Acrylates Copolymer/Hydrogenated Polyisobutene/
Phospholipids/Polyglyceryl-10 Stearate/Helianthus Annuus
(Sunflower) Seed Oil (Heliogel, Lucas Meyer Cosmetics) 2.00
Butyrospermum Parkii (Shea) Butter (Lipex 102, AAK) 2.00
Coco-Caprylate (Cetiol C 5, BASF SE) 3.00
Dicaprylyl Carbonate (Cetiol CC, BASF SE) 3.00
White Beeswax (proposed) 2.00
Dimethicone (Dimethicone, Dow Corning Corp.) 2.00
C. Water (aqua) (and) Glycerin (and) Polygonum Aviculare Extract
(Elix-IR, Lucas Meyer Cosmetics) 2.00
Water (aqua) (and) Epilobium Angustifolium Flower/Leaf/Stem
Extract (Canadian Willowherb, Lucas Meyer Cosmetics) 1.00
Vol. 134, No. 5 | May 2019 Cosmetics & Toiletries® | DE1

EXPANDED Anti-Aging Formulary
FREEZE-DRIED COCONUT ANTI-AGING B. Petrolatum 2.50

Glycyrrhiza Glabra (Licorice) Extract (proposed) 0.20
(Sabinsa Corp.) Cetearyl Alcohol (Lanette O, BASF SE) 2.50
A. Water (aqua) qs to 100.00% w/w Glyceryl Stearate (and) PEG-100 Stearate (Lipomulse 165,
Disodium EDTA 0.05 Vantage Specialty Ingredients) 2.00
Carbomer 0.35 PEG-40 Stearate 1.00
B. Polyglyceryl-3 Stearate SE 2.50 Octyldodecanol (Eutanol G, BASF SE) 2.00
Glyceryl Stearate (and) PEG-100 Stearate (Finester 1650, Dimethicone (DC 200 Fluid, Dow Corning Corp.) 1.00
Fine Organics) 2.40 Myreth-3 Octanoate 3.00
Isopropyl Myristate 1.00 Retinyl Palmitate 0.10
Tetradibutyl Pentaerythrityl Hydroxyhydrocinnamate Vitamin E Acetate 0.10
(Tinogard TT, BASF SE) 0.30 C. Citrus Unshiu Peel Extract (and) Glycerin (Melaslow PH,
C. Aminomethylpropanol (and) Water (aqua) (AMP 95, Sederma) 2.00
ANGUS Chemical Co.) 0.20 Cucumis Sativus (Cucumber) Fruit Extract 0.50
Water (aqua) 2.00 Arctostaphylos Uva Ursi Leaf Extract (Bearberry
D. Cocos Nucifera (Coconut) Fruit (Cococin, Sabinsa Corp.) 2.00 (Arctostaphylos Uva-ursi) Extract, Carrubba Inc.) 0.05
E. Phenoxyethanol (and) Ethylhexylglycerin (euxyl PE 9010, D. Citric Acid 0.35
schulke) 0.80 Preservatives qs
Cyclopentasiloxane/Phenyl Trimethicone/Dimethiconol/ Procedure: Combine A and heat to 70°C. Combine B and heat to 70°C. Add B to A
C12-15 Alkyl Benzoate/Dimethicone Crosspolymer and mix until uniform. Cool with mixing to 30°C. Add C to AB and mix well. Adjust
(Xiameter PMX 3031 Fluid, Dow Corning Corp.) 1.00 pH to 4.0-4.5 with citric acid solution. Add preservative. Homogenize for 2 min.
Procedure: Weigh all ingredients accurately. Mix first two ingredients of A, ensuring
dissolution. Add remaining A, avoiding the formation of lumps. Heat A to 70-75°C.
Heat B in oil-jacketed vessel to 70-75°C and add to A, mixing for 5-10 min. HYDRATING NIGHT FACE MASK
Homogenize emulsion, then cool to 50°C. Mix C and add to main vessel, mixing
(Shin-Etsu Silicones of America, Inc.)
well. At 50°C, add D and mix well. At 45-50°C, add E to batch and mix well.
This D5-free, leave-on, w/o gel cream mask exhibits a
fresh, water-breaking sensation that feels soothing to
SKIN LIGHTENER/WHITENER the skin and delivers intense hydration over night. The
(schülke) combination of KSG-210 and KF-6017 forms a stable
A. Water (aqua) qs to 100.00% w/w w/o cream that contains a large amount of water, which
Magnesium Aluminum Silicate (and) Cellulose Gum is the key to providing fresh and water-breaking effects.
(Veegum Plus, Vanderbilt Minerals LLC) 0.50 The high level of glycols provides intensive hydration to
Disodium EDTA 0.10 the skin without being tacky.
Xanthan Gum 10.00 A. Dimethicone/Dimethicone/PEG-10/15 Crosspolymer
Glycerin 2.00 (KSG-210, Shin-Etsu Silicones of America, Inc.) 3.00% w/w
Trimethylpentanediol/Adipic Acid Copolymer (Lexorez TL-8, Dimethicone/Dimethicone/Vinyl Dimethicone Crosspolymer
INOLEX) 2.00 (USG-110, Shin-Etsu Silicones of America, Inc.) 2.00
Kojic Acid 1.00 PEG-8 Dimethicone (and) PEG-10 Dimethicone (KF-6017,
Shin-Etsu Silicones of America, Inc.) 0.10
Dimethicone (DMF-2cs, Shin-Etsu Silicones of America, Inc.) 9.00
Blue 1 qs
B. Water (aqua) 64.50
Glycerin 10.00
Propylene Glycol 5.00
1,3-Butylene Glycol 5.00
Sodium Citrate 0.20
Sodium Chloride 0.50
Phenoxyethanol 0.70
100.00
Procedure: Combine A and mix well until uniform using a dispersing blade. In a
separate vessel, combine B and mix until uniform. Emulsify by adding B to A under
low shear (~400-900 rpm). Increase speed to ~1600 rpm for 3 min; properties:
appearance = light blue gel cream with a translucent film; viscosity, Brookfield He-
liopath RV Spindle T-C, speed 5, 1 min @ 25°C = initial @ 65,000; 24 hr @ 60,500
cps; stability: 4°C @ 3 mos = passed; 25°C @ 3 mos = passed; 45°C @ 3 mos =
passed; 50°C @ 3 mos = passed; freeze/thaw 3 cycles (-20°C @ RT) = passed.
Processing tips: Paddle mixer or disperser mixer is recommended. Homogenizer or
rotor stator homogenizer/mixer is not necessary. Elastomer should be thoroughly
mixed prior to adding other oils. The oil phase should be smooth and uniform when
properly mixed. Water phase should be added at a steady rate without “pooling.”
If pooling occurs, slow rate of water phase addition. High shear will cause the
emulsion to break. Batch requires just enough mixing/shear to ensure turnover.
Avoid storing bulk in containers with hydrophilic inner wall (i.e., glass jar). If using
glass, it should be hydrophobically treated.
DE2 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

Research | C&T ®
KEY POINTS
• An important part of the skin microbiome
is established within days of birth but
the wide use of antibiotics during labor
may disrupt the development of the
newborn microbiome.
• The clinical implication is to avoid
administering antibiotics to children, and
possibly expecting mothers, as well as to
abstain from extreme cleanliness.
Microbiome
Disconnect
M
Antibiotics and Dysbiosis: A Commentary
Ben Teoh icrobiome is becoming a household word

Ante Cosmetic
and generally refers to the mix of bacteria,
yeasts and parasites in microscopic form
Suzhou, China
in our immediate surroundings that are
invisible to the naked eye. These entities
are closely linked to everything from an
individual’s weight, mental and autoimmune health, and blood pressure,
to diabetes, heart disease and even cancer. Therefore, it is worth knowing
more about them to enhance our general well-being. In fact, bacteria are
essential for human functioning—they aid in digestion, strengthen the
immune system and help to maintain the health of our skin.
Vol. 134, No. 5 | May 2019 Cosmetics & Toiletries® | DE3
CT1905_Research_Teoh_fcx.indd 55 4/17/19 11:06 AM

Microbiome Disconnect
Limiting the bacteria microorganisms outnumber human cells by

tenfold, making the human body their home.
in the adaptive Innate Recognition Versus

immune system Antibiotics
Interestingly, researchers at the University
early can be linked of California, San Francisco, have found that
to autoimmune
an important part of the skin microbiome is
established within days of birth, with a large
and inflammatory amount of T-cell activity creating tolerance in

the immune system to the bacteria living on
diseases later in life. the skin. This is a critical factor in the immune
system’s understanding—to stop attacking the
normal and healthy bacteria on the skin.
However, the wide use of antibiotics during
As the largest organ, skin takes up a surface labor may unintentionally disrupt the develop-
area of approximately 1.8 m2. It protects us ment of the newborn microbiome and cause
from the environment, serves in thermoregula- dysbiosis, which could in turn lead to a rise
tion and of course, is key for our appearance. in skin-related disorders that are difficult to
The skin’s own microbiome is an ecosystem remedy later in life as an adult.
of 10 to 100 trillion organisms; in fact, these Clearly, the clinical implication is to avoid
administering antibiotics to children—
and expectant mothers, if possible—in
the early neonatal stages because this
will limit the amount and type of
bacteria present in the adaptive immune
system, which can be linked to the
development of autoimmune and inflam-
VIDEO matory skin diseases later in life. These
findings also suggest it may benefit
A Probiotic-like Approach
an infant’s microbiome by abstaining
from bathing them for the first few days
to Skin Care
of life.
In contrast, hygiene and dietary
habits are the main approaches to help
adults improve the negative effects of
dysbiosis, ultimately giving rise to a
normalized skin appearance.
Truth in Tradition
The described findings may bring to
light the source of an ages-old Chinese
tradition forbidding nursing mothers to
wash themselves thoroughly before the
lapse of three to four weeks after birth,
somewhat vindicating advice against
measures to achieve extreme cleanliness/
tidiness. This advice is understood to
be applicable to newborns as well and
hopefully will earn due consideration
as a special mention in product efficacy
claims or advertisements, as well as
formulas targeting these users.
DE4 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019
CT1905_Research_Teoh_fcx.indd 56 4/17/19 11:06 AM

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As we
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10 [video] How Muscle Controls

DE3 Microbiome Disconnect

DE4 [video] A Probiotic-like Approach

48 34 Testing Tactics in Skin: Total Breakdown

37 [video] Hyaluronan Homeostasis for

2 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

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Discover HyWhite and other active

Top European quality of anti-aging ingredients

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Partner & CEO George Fox

OTHER ALLURED PRODUCTS

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sensiva® multifunctional additives promote the

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6 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

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Flexing Beauty Biceps: How Muscle

SN: My research was about muscles of the body. We found a

Marc Pissavini, Ph.D. C&T : What did you discover?

Luigi Rigano, Ph.D. which is secreted from muscle,

Peter Tsolis to apply this research?

SN: I think the next step is

Russel Walters, Ph.D. product development, such as

10 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

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More information is available at: www.wacker.com/belsileco www.wacker.com/socialmedia

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Skin Care Solvers

12 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

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SpectraFlex Illusion Pigments

Natural and Sustainable

InstaMask Shale with

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14 | www.CosmeticsandToiletries.com Vol. 134, No. 5 | May 2019

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Antioxidant and Probiotic Solutions

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• The present article reviews research related

Picking Up the Slack

Katerina Steventon, Ph.D.

Reproduction in English or any other language of

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October 15, 2019

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and positively to the elastic recovery from

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Vol. 134, No. 5 | May 2019 Cosmetics & Toiletries® | 19

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• Safety is a major consideration when

• This article describes safety guidelines in

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