Cosmeticsandtoiletries201510 DL PDF

October 2015
Biomimetic vs.
Traditional Skin
Moisturization p 30
W/O/W Technology to Enwrap Sunscreens p 16
Measuring Yield Stress in Personal Care p 44
Skin Directory p 60
Focus
Skin
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C&T October 2015 Editor’s note | C&T
Cover art by James Fergus
2 Editor’s Note
6 Scientific Advisors
64 Advertiser Index Kevin Campbell
A regulatory wave
Market Intelligence Wow. What a year for regulations in the cosmetics industry, eh?
First it was the Personal Care Product Safety Act, aka the
8 Driven by Innovation and Expansion into Feinstein Bill, making it into Congressional Committee back in
Emerging Markets: Transformation in April, where it currently resides while the lawmakers debate.
Body Care by N. Tyrimou Then it was animal testing bans in Turkey. And right on the
heels of that, animal testing bans in Russia.
10 Technology Launches And now comes some good news. As Nicole Urbanowicz,
C&T associate editor, reported online, California Superior Court
for Alameda County this summer ruled in favor of the cosmetics
Regulatory industry in a case concerning the use of titanium dioxide. The
lawsuit, brought before the court by the Public Interest Alliance,
12 Navigating the Ever-Changing was decided on summary judgement based on lack of evidence by
Regulatory Landscape in China, Part II the plaintiff.
by K. Yarussi-King Dealing with regulations in Europe and other parts of the
world has been an ongoing process over the years. But in North
America—and primarily in the United States—where legislation
Research has changed little since the turn of the 20th Century, it has been
less of a concern. Until now.
16 W/O/W Technology to Enhance Get ready, folks. This is just the beginning.
Organic UVA/UVB Sunscreen Performance As we have seen this year, legislative bodies the world over are
by E. Wang, D. Chen and K. West acting more frequently, and often more aggressively, on regulatory
issues. Why that is depends on each individual issue of course,
26 What do We Know About but the special interests like the Public Interest Alliance are always
Depigmenting Agents? by S. Saxena, stirring the pot. The moment they hear of something that can
R. Andersen, M.D., and H.I. Maibach, M.D. further their cause they attack it. And we all know the approach
they take is rarely a scientific one.
30 An In vivo Comparison of That’s just one more reason that this time in cosmetic science
Biomimetic vs. Traditional Skin Moisturization is so important. Your role as a cosmetic scientist, whether you’re
by P. Todorova, P. Grant-Ross, S. Tamburic in formulations, research or testing, has never been more critical.
and R. Kurimo Not only are you researching and developing new products to grow
business, you’re also on the front line to ensure those products meet
the standards that are set, and that they can be defended when the
Testing public interest sharks start to circle.
As a scientist, it’s so difficult to stand by while the special
44 Yield Stress Measurements for interest groups make the rounds in the news, on the talk shows and
Personal Care, Part I: Definitions and Basics on the Internet. They often succeed at making lots of noise that can
by J. Martin, Ph.D. distract from the real issues. But they often fail to have scientific
information to back up their claims. That’s something you have,
and that you produce every day.
Formulating The coming wave of regulations is just beginning to swell; there’s
little stopping it. But it’s the data you generate in your lab that will
58 Sponsored–Silab: Biotechnologies: Another carry the industry through the regulatory storm.
Outlook on Mastering Nature by SILAB
60 Skin Directory
2 | www.CosmeticsandToiletries.com Vol. 130, No. 8 | October 2015

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Scientific Advisory Board | C&T
“Given today’s active lifestyle, future innovation in recreational sunscreen will focus
on high-performance situations (beach, sports) without losing efficacy or trading off
aesthetics. Opportunity also exists to create smart sun technologies that can provide
consumers feedback on ideal sunscreen formulas and application in real-time, at point-
of-purchase or during use.
Prithwiraj Maitra, Ph.D.

Johnson & Johnson
Eric Abrutyn Shuzo Ishidate, Leslie C. Smith,

TPC2 Advisors Ltd. Ph.D. Ph.D.
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Center
Zoe Diana Jennifer Marsh, David C. Steinberg

Draelos, M.D. Ph.D. Steinberg & Associates
Dermatology Procter & Gamble
Consulting Services
Angela R. Eppler, Marc Pissavini, Peter Tsolis

Ph.D. Ph.D. The Estée Lauder
Pfizer Consumer Coty-Lancaster Companies
Healthcare
Trefor Evans, Ph.D. Luigi Rigano, Ph.D. Russel Walters,

TA Evans LLC Industrial Consulting Ph.D.
Research Johnson &
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S. Peter Foltis Sylvianne Xiao Wu, Ph.D.

L’Oréal Schnebert, M.D. Eli Lilly and Co.
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Market Intelligence | C&T
Driven by Innovation and Expansion

into Emerging Markets:
Transformation in Body Care
Nicole Tyrimou, Euromonitor International
W
hile facial care continues to account
for the lion’s share of skin care total
value sales, body care has been going Body Care
through a transformation period, driven by
n Individual consumers
innovation and further expansion into emerg- spent an average of U.S.
ing markets. $2.50 on body care in 2014.
Body care remains a low priority in
spending for consumers globally compared n Western Europe and
to facial care, with individual consumers North America beauty
spending an average of U.S. $2.50 on body companies turned to
care in 2014, compared to more than U.S. $12 innovation to rejuvenate the
on facial care. body care category.
However, body care’s great importance
to beauty companies stems not only from n A key traditional
Western Europe holding a significant share consumer complaint about
of its premium sales (42% in 2014), but also body care offerings is the
from its strong growth in the Middle East, amount of time it takes for
Africa and Latin America—at just under application and absorption
10%—in 2014. of the product.
Convenience and n Improvements on the body care product experience

include lighter, faster-absorbing formulations, exotic
Customization fragrance and luxurious texture.
While body care continues to show stable
growth in Latin America, the Middle East and n Firming and anti-cellulite body care grew by 1.6%
Africa, Western Europe and North America globally in 2014, despite continued declines in Western
beauty companies turned to innovation to and Eastern Europe as well as North America. The Middle
rejuvenate the category. East, Africa and Latin America lead growth in the body
A key complaint consumers traditionally care category.
have about body care offerings is the amount
of time it takes for application and absorption n One of the key obstacles to body care’s growth
Save to of the product. This has been a key focus for prospects remains the low penetration in the dominant skin
My Library companies, which have targeted convenience care region of Asia Pacific.
as a way to add value to body care offerings.
Reproduction in English or any other language of

8 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 130, No. 8 | October 2015
© 2015 Allured Business Media.
Being viewed as a timely and secondary part of a luxurious experience for consumers, which may
the skin care routine can drop a product down or off persuade them to skip the body moisturizer.
consumers’ shopping lists. Finally, one of the key obstacles to body care’s
Beiersdorf emphasized in its first-half results growth prospects remains the low penetration in the
presentation that its new launches, including the In- dominant skin care region of Asia Pacific. In Asia
Shower Body Care line, which has been expanded to Pacific, where over half of total skin care value sales
six products, including In-Shower After Sun and Q10 are generated each year, body care remains of low pri-
Firming Body Lotion, have been recording double- ority, as culturally, consumers are more accustomed
digit growth. The company also stressed the Nivea to spending on multi-step, complex facial regimes
Express Hydration line reaffirms the brand’s commit- than on any body care offering.
ment to creating convenient products for consumers. However, body care offerings with added proper-
Beyond convenience, skin care brands have ties, such as whitening, have helped push the category
also invested in developing more sophisticated and forward and Asia Pacific is expected to be the biggest
customized body care offerings for consumers similar contributor to body care’s absolute value growth over
to those found in facial care. Customization has been 2014-2019, adding half a billion dollars to its value.
visible in order to add value to body care offerings, Continuing penetration into this region, especially to
with brand owners segmenting their ranges to create capture new consumers, will be pivotal to body care’s
more personalized solutions to groups of consumers. future global growth prospects.
Creating an Experience
Body care brand owners are also working on
improving the experience of their products through
lighter, faster-absorbing formulations as well as look-
ing to create a more pampering experience through
exotic fragrance and luxurious texture.
These launches aim to glamorize the basic body
care category and create a positive experience around
the application of body care offerings using scent
and texture.
Furthermore, the introduction of leggings, jeans
and underwear with skin care properties (commonly
known as cosmotextiles) is a further example of trying
to create a better experience for consumers, especially
for firming and anti-cellulite products.
Firming and anti-cellulite body care grew by
1.6% globally in 2014, despite continued declines
in Western and Eastern Europe as well as North
America. The Middle East, Africa and Latin America
lead growth in this category, as in general body care.
Nivea and Mixa have been introducing leggings
and shorts with anti-cellulite properties to provide
consumers with an alternative experience in using
these products. The introduction of moisturizing
cream in jeans by Wrangler and in underwear by
Triumph two years ago was also aimed at providing
a more luxurious experience for consumers while
wearing their products.
Future Challenges
Dove’s latest beauty makeover campaign show-
cases neither a skin care nor a color cosmetics
product, instead being about body shower. This illus-
trates the potential power of body shower products
with moisturizing properties and how they can create
Vol. 130, No. 8 | October 2015 Skin Cosmetics & Toiletries® |9

Market Intelligence | C&T
Technology Launches
repairing moisturizer lIGHTENING EMULSIFIER
Silab’s Nerenyl (INCI: Saccharide Dermofeel Easymuls Plus
Hydrolysate) ingredient stems from (INCI: Glyceryl Oleate
the ancestral African locust bean Citrate) by Dr. Straetmans is a
tree, or Parkia biglobosa, which is second-generation emulsifier
characteristic of the West African for low viscous emulsions.
savanna. The plant is recognized for The ingredient is best suited
its ability to resist dryness. to spray applications and is
This ingredient has the ability applicable for cold processing.
to strengthen the skin barrier and In addition, the company’s Dermofeel Enlight (INCI:
moisturize skin. One in vivo study proved the ingredient enabled Water (Aqua) (and) Sodium Phytate (and) Glycerin (and)
the recovery of skin barrier function in just four days, as opposed Morus Alba Fruit Extract) is a natural ingredient, designed
to seven with the placebo. for efficient skin whitening. Proven in vivo, the material
Another in vivo study showed after 28 days of twice daily incorporates phytic acid and mulberry extract for natural
application, the ingredient formulated at 3% in an emulsion age-spot correction.
significantly smoothed the crow’s feet area microrelief as well as www.dr-straetmans.de
improved complexion radiance parameters.
www.silab.fr
revitalizing offerings
CM-Glucan Forte (INCI:
Magnesium Carboxymethyl
Beta-Glucan) by Mibelle
Biochemistry is a modified
polysaccharide developed
from the cell walls of baker’s
yeast. The ingredient soothes
skin prone to irritation such as
eczema. It also helps to shift the
response of pathogens toward
the Th1 immune response
pathway, rebalancing skin to help suppress overreactions to
allergens resulting in itchy, red and dry skin.
Vin-UpLift (INCI: Not Provided), also by Mibelle,
is designed to lift skin, reducing wrinkles and fine
lines. Derived from ice wine, which contains higher
concentrations of polysaccharides and polyphenols, the
ingredient is spray-dried onto a carrier polysaccharide from
Caesalpinia spinosa (tara gum), producing an alcohol- and
preservative-free compound. In a placebo-controlled study,
a cream containing the ingredient was shown to instantly
lift and tighten skin, while decreasing wrinkle depth within
30 min after application.
www.mibellebiochemistry.com

Regulatory | C&T
Navigating the Ever-Changing

Regulatory Landscape in
China, Part II
Karen Yarussi-King
Global Regulatory Associates, Inc.
Raleigh-Durham, N. Carolina
E
arlier this year (C&T January/February 2015), I provided an update to
KEY WORDS the dynamic regulatory environment in China. Well, true to form, the
Chinese government has again surprised the cosmetic industry in the
regulation • China • Asia • latest draft of its cosmetic regulations.
Chinese • food • drug • Various trade associations, including the Personal Care Products Coun-
administration • CFDA • cil and Cosmetics Europe, worked with the U.S. government and World
formulating • ingredient Trade Organization to address industry concerns with the Chinese Food
labeling and Drug Administration (CFDA).
In an amazing twist, the Chinese government has been receptive to the
feedback from the global cosmetic industry on their previous draft. The
latest draft of the Cosmetics Supervision and Administration Regulations
(CSAR) resembles a more Western approach to regulating the cosmetics
ABSTRACT
industry but, of course, with a Chinese twist.
In an unlikely turn, the
Chinese government has Raw Materials
embraced a Western The CFDA will now issue catalogs of prohibited, restricted and
approach to cosmetics permitted ingredients, updated on an annual basis. The model will be
regulation. However, it similar to the EU Annexes. Previously, industry could only choose from
ingredients on the approved positive list, which was not regularly updated
comes with a traditional
to include innovations in raw material technology, particularly with skin
Chinese twist. care ingredients.
As a result, many cosmetic manufacturers were forced to provide dif-
ferent formulas designed specifically for China. This development will help
cosmetic manufacturers by allowing for a single global formula, which in
turn, will hopefully provide economies of scale production savings.
It appears the CFDA also has changed its thinking on adding new
ingredients to the permitted catalog. While clarity is still being sought, new
ingredients not considered to be high-risk can be added by the manufac-
turer of a domestic product or agent of an imported product within 30 days
of its use in the manufacturing process. This allows manufacturers or agents
to place a product on the market immediately after the ingredient’s listing.
In addition, the manufacturer or agent will need to report on the use and
Save to
safety of new ingredients semi-annually for their first three years of use.
My Library
The cosmetics industry is also asking that raw material manufacturers be
permitted to apply, since they are the primary source of ingredient data.

Regulatory | C&T
Finished Products Special cosmetics must be registered before being
The CFDA has divided products into two cat- manufactured domestically or imported, and will
egories: special and ordinary cosmetics. The Chinese require the same documentation as ordinary cosmet-
government will create a catalog of special cosmetics ics with the addition of the product formulation.
that manufacturers will be able to review to deter- What remains undefined is whether existing safety
mine if their product is considered a special cosmetic. assessments can be used as support in China.
Currently, special cosmetics include hair dyes,
perms, whitening products and sunscreens, as well
Labeling
as other cosmetics considered to require special Earlier this year, as part of this regulation, the
administration—although authorities of the state CFDA proposed the prohibition of over-labeling.
council have not yet defined what criteria would This would have meant entire product labels would
cause a product to require special administration require printing in Chinese, forcing cosmetic compa-
categorization. Any cosmetics falling outside of the nies to prepare and manage a separate inventory for
special criteria are classified as ordinary. China. To the non-Chinese cosmetic industry, this
It appears the notification process for ordinary could lead to consumer confusion over the origin
of the product because it would
not necessarily look like a typical
foreign product the consumer was
The most recent version of accustomed to purchasing.
CSAR does show a real attempt The rationale was that, under
the current regulation, only the
by the Chinese government mandated information needs to
be presented in Chinese—name
toward harmonization with the of product, name and address of
distributor/manufacturer, ingre-
rest of the world. dients, etc.—and could be added
to a package with an over-label.
However, this also allowed English
cosmetics will be greatly reduced from what claims, depending on the label
previously required months, to just 10 days. The configuration, to be visible. And if the over-label were
Chinese government must be notified of new removed, it could lead to a perceived competitive
domestically produced products 10 days before their advantage over domestic Chinese brands.
manufacturing begins. The government must also be In the latest version of the CSAR, over-labeling
notified of imported products 10 days prior to their is acceptable if the “sticking” process meets quality
being imported. management standards for cosmetic manufactur-
The following documents must be provided for ing. The over-label must also be provided during
notification to the CFDA: the registration/notification process. Therefore, it
• contact information for the agent and/or manu- seems safe to say the label will be required to be
facturer of the product, permanently affixed to the packaging and difficult to
• product name and full ingredient list, intentionally remove.
• national or enterprise standards applied to Over-labels will need to be presented in standard-
the product, ized Chinese characters. If the label contains other
• test reports, characters, they must be consistent with standardized
• safety assessment and Chinese characters. Further, the content of the labels
• product label and other technical data, including “shall be truthful, complete and accurate.” While this
GMP certification and evidence that the product is vague and will need clarification, it is good news
is being sold in the country of origin. for the industry that over-labeling is permitted under
the latest draft of the CSAR.
The following data must be supplied on the over-
label, in Chinese:
Market Intelligence • name of the product,
• name and address of the manufacturer (brand),
n It is estimated the Chinese cosmetic market
• name and address of the manufacturing com-
could be worth as much as US $13 billion or more.
pany (brand or third party manufacturer),
Source: www.CosmeticsandToiletries.com • manufacturing license number of the manufac-
turing company (except for imported cosmetics),

• registration license number of special cosmetics literature can be used to substantiate the claimed effi-
or notification number of ordinary cosmetics, cacy unless the CFDA deems it necessary to conduct
• standards codes the product conforms to, testing; as of now, this, too, is undefined.
• full ingredients list, All relevant literature, research data or efficacy
• shelf-life, substantiation will now need to be added to the
• net weight, CFDA website for consumer review and acceptance—
• warnings (if necessary), and yes, the Chinese twist. With the technical nature of
• any other contents to comply with additional claims support, this could very well spell disaster. The
laws, regulations or requirements of the CFDA. global cosmetic industry will, without a doubt, fight
this provision.
Claims Support The most recent version of CSAR does show a real
In addition to the draft cosmetic regulations, the attempt by the Chinese government toward harmo-
CFDA issued a draft Administrative Management of nization with the rest of the world; however, we will
Cosmetic Labeling, which includes a provision that have to wait for the final verdict until more details
claims must be validated by an independent third- emerge in the coming months.
party in China before they can be placed on the label.
This would require companies adding efficacy or
performance claims to their product’s labeling to have
their claims pre-approved before submitting artwork
for registration.
While the process is not yet defined, the CFDA
is now requiring efficacy claims be based on “suf-
ficient” scientific data, placing the responsibility for
the claimed efficacy on the manufacturer. Scientific
Vol. 130, No. 8 | October 2015 Skin Cosmetics & Toiletries® | 15

Research | C&T
W/O/W Technology to
Enhance Organic UVA/UVB
Sunscreen Performance
Eric Wang and Delphine Chen
Bio-Nest Biochemical Technology Co., Ltd., Taiwan
Keith West
Kuo Ching Chemical Co. Ltd., Taiwan
T
he sunscreen market has long been dominated by sun care products
KEY WORDS using organic UV filters. However, incorporating these chemical
actives into formulae intended for day-long wear is a concern. One
w/o/w • SPF • dispersion problem is they can cause skin irritation in some consumers. What’s worse,
aggregation • penetration some people become sensitized to certain UV filters, and there is no guide-
photostability line for avoiding the irritation problem beforehand.
Another challenge is the tendency of UV filters to aggregate, which
can reduce their SPF performance despite increasing their use levels. To
overcome this problem, formulators may mix four to six different UV filters
ABSTRACT
in the formula for a total concentration of no less than 18% to produce an
A new water-in-oil- SPF 50 sunscreen. Such a high level of sunscreen and variety of UV filters in
in-water technology one formula inevitably increases the risk of skin irritation.
is described here that Considering these challenges, a specialized water-in-oil-in-water
functions as an isolating (w/o/w) system was developed to function as an isolating shield, enwrap-
shield, preventing UV filter ping UV filter particles to prevent them from aggregating while at the
same time helping their dispersion. With the aggregation problem solved,
particles from aggregating
SPF performance is greatly enhanced, as is shown here. Further, effi-
and helping their
ciency is improved since lower levels of UV filters are required to provide
dispersion in formulas. higher SPFs.
By enwrapping chemical
sunscreen agents, the W/O/W System
technology is shown in To prepare the system, a proprietary, high pressure and high shear
vitro and in vivo to improve process is used to control the particle size of the pre-solubilized mixture
SPF performance, UVA/ of both liquid and powder chemical sunscreen at micron meter levels. The
UVB wide band high sunscreen mixture is then encapsulated in a w/o/w double sphere system,
which stabilizes the chemical sunscreen content and converts it into an
protection ratio, SPF
aqueous dispersion (see Figure 1). This unique double sphere structure has
sustainability and safety a lipophilic active ingredient, such as a chemical UV filter, enwrapped in the
concerns regarding skin outer layer. In addition, the hydrophilic active ingredient is enwrapped in
penetration. the inner core.
SPF In vitro
To assess the capabilities of the w/o/w technology, two sunscreen
Save to
combinations were formulated with the system for SPF testing. The first was
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a combination of ethylhexyl methoxycinnamate (20%), octocrylene (10%)
and butyl methoxydibenzoylmethane (20%)a. The second incorporated

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Research | C&T
ethylhexyl methoxycinnamate (25%), benzophenone-3 UVA Protection
(10%) and butyl methoxydibenzoylmethane (15%)b. The UVA protection capability achieved by each
Both combinations were added at different percentages formula containing the w/o/w system, as determined
into a gel (see Formula 1) and cream (see Formula 2). following the Boots Star Rating system, also was
SPF performance was measured using a UV outstanding, as shown in Table 3 on Page 20. Almost
transmittance analyzerc, the results of which are shown all formulas achieved the highest UVA protection
in Table 1. As can be seen, just 10% of either sunscreen possible, except the first blenda at its lowest percent-
blend was required in the final formulae to achieve an age. Besides the cream and gel formulas presented
SPF of 50 or more—even up to 70, in the case of the here, the w/o/w system has been incorporated into
By treating sunscreens Market Intelligence

with the w/o/w system, n In 2014, sun care’s global retail value grew
at its slowest pace in a decade, according to
the SPF increased by Euromonitor International. North America and
eight to 11 times. Western Europe were flat but the category was
bailed out by demand in Latin America, where
sales climbed 18% at fixed U.S. dollar exchange
rates to $2.3 billion. However, spending power
first blend in a gel formula. Further, when UV filter will likely tighten significantly, meaning there is
combinations were incorporated in the cream with 3% little room for complacency among global sun
titanium dioxide, the SPF performance was boosted care brands.
dramatically; the cream formula with TiO2 is shown in
Formula 3 on Page 20, and the respective SPF perfor- Source: GCI (GCImagazine.com)
mance is shown in Table 2, also
on Page 20.
The cream with 3% TiO2 Figure 1. Schematic of w/o/w double sphere system
alone yielded an SPF of only
4.88, compared with the blank
cream having no sunscreen
actives, which provided an SPF
of 1.63. However, when 3% of
the firsta or secondb sunscreen
blend was added to the cream,
the SPF performance increased
from 8 to 11 times, easily
achieving an SPF of 50 and 30,
respectively. This was with a
total concentration of organic
and inorganic sunscreen actives
at just 4.5%. Such synergistic
effects have never before
been observed.
Formula 1. Test gel
a
SunCat MTA (INCI: Water (aqua) (and) Water (aqua) qs
Ethylhexyl Methoxycinnamate (and)
Butyl Methoxydibenzoylmethane (and) Triethanolamine 0.03% w/w
Octocrylene (and) Phospholipids (and) Glycerin 5.00
1,3-Butylene Glycol) and Carbomer (2%) 15.00
b
SunCat DE (INCI: Water (aqua) (and)
Phenoxyethanol 0.10
Ethylhexyl Methoxycinnamate (and)
Butyl Methoxydibenzoylmethane (and) Water (aqua) (and) Ethylhexyl Methoxycinnamate (and) Butyl
Benzophenone-3 (and) Phospholipids Methoxydibenzoylmethane (and) Benzophenone-3 (and)
(and) 1,3-Butylene Glycol), Bio-Nest Phospholipids (and) 1,3-Butylene Glycol) (SunCat DE,
Biochemical Technology Co., Ltd.
Bio-Nest Biochemical Technology Co., Ltd.) qs
c
UV-1000S Ultraviolet Transmittance
Analyzer, Labsphere

other formulae to test for SPF performance. All UVA-PF In vivo
showed remarkable and reproducible SPF results; the UVA-PF in vivo testing also was performed, in
results of another cream formula including 3% TiO2 accordance with the Declaration of Helsinki and
are presented later in this article. national regulations regarding human studies as
Formula 2. Test cream

Polyglyceryl-3 Methylglucose Distearate (Tego Care 450, Evonik) 4.50% w/w
Cetearyl Alcohol 1.00
Bio-Squalane (lighter) (NeSol 2902b, Bio-Nest Biochemical Technology Co., Ltd.) 14.50
Propylene Glycol 7.00
Euglena Gracilis Polysaccharide 5.00
Water (aqua) qs
Phenoxyethanol 0.12
Water (aqua) (and) Ethylhexyl Methoxycinnamate (and) Butyl Methoxydibenzoylmethane (and)
Benzophenone-3 (and) Phospholipids (and) 1,3-Butylene Glycol) (SunCat DE,
OR
Octocrylene (and) Phospholipids (and) 1,3-Butylene Glycol) (SunCat MTA, Bio-Nest
Biochemical Technology Co., Ltd) qs
Table 1. SPF Performance of Each Preparation
W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

First blend gel
a
1.57 13.39 22.54 44.12 51.66 52.00 54.02 57.26 72.98
First blenda cream 1.63 21.26 32.53 41.10 46.04 46.82 48.26 51.89 53.15
Second blenda gel 1.57 12.13 19.07 33.79 38.39 52.29 52.48 52.27 58.39
Second blend a
1.63 13.56 22.62 24.08 31.97 33.58 41.23 43.82 52.20
cream

Research | C&T
described by International Standard ISO 24442. wavelengths or energy-shedding by photochemical
Similar in vivo results were obtained to those found processes; for example, isomerization and heat release.
in vitro (see Table 4 on Page 22). Thus, when interacting with UV radiation, organic UV
filters undergo a degradation process and lose their UV
Photostability protection ability. This is why product labels remind
As is generally known, organic UV filters provide consumers to reapply sunscreen every few hours—to
sun protection with more a comfortable skin feel than maintain protection.
inorganic sunscreens. However, their UV-absorbing In relation, an after-sun-exposure SPF study was
mechanism also flaws their protective capabilities. As conducted to determine whether the UV absorbance
Gago-Ferrero et al. explain,1 organic UV filters absorb rate of the w/o/w system decreases after being exposed
radiation with excitation to a higher energy state. This to UV light. The firsta sunscreen blend was incorpo-
excess energy is dissipated by the emission of higher rated in a cream base at 5% and 7%; in a gel base at 8%
Formula 3. Test cream plus 3% TiO2

Polyglyceryl-3 Methylglucose Distearate (Tego Care, Evonik) 4.50% w/w
Cetearyl Alcohol 1.00
Bio-Squalane (lighter) (NeSol 2902b, Bio-Nest Biochemical Technology Co., Ltd.) 14.50
Titanium Dioxide (and) Talc (and) Dimethicone (Nestdry ST-2000, Bio-Nest Biochemical
Technology Co., Ltd.) 3.00
Propylene Glycol 7.00
Euglena Gracilis Polysaccharide 5.00
Water (aqua) qs
Phenoxyethanol 0.12
Benzophenone-3 (and) Phospholipids (and) 1,3-Butylene Glycol) (SunCat DE,
OR
Octocrylene (and) Phospholipids (and) 1,3-Butylene Glycol) (SunCat MTA, Bio-Nest
Biochemical Technology Co., Ltd) qs
Table 2. SPF Performance with 3% TiO2
W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

First blend a
4.88 55.12 61.34 66.47 68.49 73.86 76.23 76.64 80.43
Second blend a
4.88 33.88 59.15 57.82 62.27 75.30 83.86 89.34 95.61
Table 3. UVA Protection for Each Formula
W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

First blend gel
a
* ** **** **** **** **** **** **** ****
First blend cream
a
** **** **** **** **** **** **** **** ****
First blend cream
a
**** **** **** **** **** **** **** **** ****
+ TiO2
Second blenda gel **** **** **** **** **** **** **** **** ****
Second blend a
**** **** **** **** **** **** **** **** ****
cream
Second blenda
**** **** **** **** **** **** **** **** ****
cream + TiO2

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Research | C&T
and 10%; and another cream at 3% and 5% that also Results, shown in Table 5, indicated the w/o/w
contained 3% TiO2. The slides to which each sample technology prolonged the protective effects of the
was applied were exposed to natural sunlight in the chemical UV filters. The SPF of each formula includ-
southern part of Taiwan, at noon, for up to 6 hr. After ing the w/o/w technology decreased very little, even
sun exposure, the SPF protection of each was tested. after 6 hr of sun exposure. And comparing the data in
Table 4. UVA-PF Test Results (ISO-24442, in vivo)

In vivo UVA-PF Cream base Gel base Cream + TiO2
First blenda w/w % 5% 10% 3%
UVA-PF value 17.9 18.3 19.2
UVA-PF PA ++++ PA ++++ PA ++++
Table 5. SPF Before and After Sun Exposure
Cream base Gel base Cream + TiO2

First blend w/w %
a
5% 17% 8% 10% 3% 5%
Before sun exposure SPF 31.86 51.36 42.60 48.39 57.36 63.50
After 2 hr exposure SPF 36.35 46.81 45.59 51.39 63.91 73.11

Research | C&T
Table 3 with Table 5, the SPFs of the TiO2 cream
were raised to 20~40 higher than those cream Figure 2. Franz cell schematic
formulas without 3% TiO2. Although the exact
mechanism of this protection-prolonging effect is
still unknown, this technology presents interest-
ing potential for application with chemical
UV filters.
Percutaneous Absorption
As noted, one drawback to organic UV filters
is they can cause skin irritation, potentially
deterring the user from using products containing
them. This irritation occurs because organic UV
filters in conventional preparations can penetrate
the skin and reach the capillaries.2-4 In response,
the body’s natural defense system is initiated
and reacts to the alien UV filter with rashes
and swelling.
Formulators have spent long hours try-
ing combinations of UV filters to reduce the
potential for allergic reactions. In relation, the Figure 3. UV-absorbing capabilities in w/o/w-
results of a percutaneous absorption study with treated OMC (a) vs. OMC alone (b)
this w/o/w technology, described here, show it
could solve such problems. The test was carried
out following OECD guideline 428 with some
modifications.5 Franz cells (see Figure 2) and
non-viable skin were used for mimicking skin
absorption physiology.
Three cream samples were formulated based
on cetyl alcohol, hydrogenated poly-1-decene,
polyglyceryl-3 methylglucose distearate, Euglena
gracilis polysaccharide, phenoxyethanol, 3-iodo-
2-propynylbutylcarbamate and propylene glycol.
One additionally contained octyl methoxycin-
namate (OMC) alone; another contained OMC
with the w/o/w system; and the third blank
cream included no UV filters. All samples were
applied on non-viable skin and left for 24 hr in a
36.6°C environment.
After incubation, the buffer solution from the
Franz cell receptor chamber was drawn off to test
its UV-absorbing capabilities. Figure 3 shows the
buffer solution drawn from the w/o/w-treated
OMC chamber had much less UV-absorbing
capability than OMC alone. Interestingly,
although the buffer solution in the OMC + w/o/w
chamber showed trivial UV-absorbing capabili-
ties, its curve was almost identical to the solution
drawn from blank-cream chamber (see Figure 4).
This shows the minimal UV-absorbing capa-
bility was likely from other ingredient(s) in the
cream base. From the results of this percutaneous
absorption study, the w/o/w technology was
found to provide a strong propensity for reducing

UV filter absorption
into the skin, hence Figure 4. UV-absorbing capabilities in w/o/w-treated OMC cream (a)
reducing the irritation vs. blank cream without UV filters (b)
potential of the chemi-
cal sunscreen.
In vivo Skin
Irritation/
Sensitization
A third partyd
tested the firsta w/o/w
system for skin irrita-
tion and sensitization
using a repeated insult
patch test (RIPT).
Fifty-two subjects,
ages 20-67 and
including nine men
and 43 women, were enrolled. Results (not shown) safer formulation, meeting the challenges faced by
indicated the sample was a non-primary irritant and formulators and resulting in big benefits for the users
non-primary sensitizer to the skin. of sunscreen products.
Conclusion References
Despite the popularity of UV filters used in sun 1. P Gago-Ferrero, MS Diaz-Cruz and D Barcelo, An overview of
protection products, they still present challenges UV-absorbing compounds (Organic UV Filters) in Aquatic Biota,
Anal Bioanal Chem 404 2597-2610 (2012)
the industry has yet to address. The practicability of
2. Z León González, Percutaneous absorption of UV filters
incorporating this new w/o/w form of UV filters has contained in sunscreen cosmetic products: Development of
been widely proven, and its successful implementa- analytical methods, Springer Theses (2014)
tion into formulations welcomed by formulators. 3. H Gonzalez, A Farbrot, O Larkö and A-M Wennberg, Percutane-
ous absorption of the sunscreen benzophenone-3 after repeated
The most difficult challenges can now be resolved whole-body applications, with and without ultraviolet irradiation,
by remarkably enhancing the performance of Brit J Derm 154(2), pp 337–340 (2006)
well–accepted, existing organic UV absorbers. Such 4. GJ Nohynek and H Schaefer, Benefit and risk of organic ultra-
“old” materials are thereby renovated for easier and violet filters, Regulatory Toxicology and Pharmacology 33(3) pp
285-99 (2011)
5. OECD, Skin absorption: In vitro method, Guideline 428, Guide-
d
AMA Labs lines for the Testing of Chemicals, Paris (2004)

Research | C&T
What do We Know About

Depigmenting Agents?*
Sparsha Saxena, Rosa Andersen, M.D., and
Howard I. Maibach, M.D.
University of California, San Francisco, CA
H
yperpigmentation is a disorder caused by the overproduction of
KEY WORDS melanin. Common hyperpigmentary disorders include, but are not
limited to, post-inflammatory hyperpigmentation (PIH), melasma
hyperpigmentation •
and solar lentigines or sun spots.1 PIH results from excess pigment that
hydroquinone • clinical evolves after trauma such as burns, acne, allergies2 and others. Melasma,
trial • safety • efficacy also known as cholasma, looks like patches of tan skin around the cheeks
skin care and face. It has numerous causes, including sun exposure, and hormonal
changes during pregnancy or associated with hypothyroidism.3
Laser treatment, chemical peels and systemic therapy are available to
treat hyperpigmentation but topical depigmenting agents are popular,
ABSTRACT convenient options. Hydroquinone, the most widely used depigmenting
This review examines the agent, was discovered in the late 1930s after its monobenzyl ether was found
efficacy and tolerability to be depigmenting workers’ skin in a rubber factory.
of agents such as Hydroquinone has been used alone for treatment but over time, its
hydroquinone, ascorbic efficacy has been improved when combined with other agents;4 Kligman
et al., for example, combined 0.1% tretinoin, 5% hydroquinone and 0.1%
acid and retinol to treat
dexamethasone.2 While hydroquinone was successful for depigmenta-
hyperpigmentation tion, however, the European Union banned it in 2001 due to harmful side
disorders. The authors effects, including exogenous ochronosis, leukoderma en confetti, and
assess the quality of possible carcinogenicity.4
studies as a tool to In response to hydroquinone’s toxicity, efforts to shift toward alternative
determine efficacy of depigmenting agents such as kojic acid, licorice extract, niacinamide, azelaic
depigmenting agents. acid, etc., have been under way. In consideration of the many ingredients
Along with outcome, they having potential depigmenting effects, the authors sought to understand
whether these agents are more tolerable and effective than hydroquinone.
also analyze study design,
The present work describes their investigation.
participant skin type,
Assessing the quality of studies is one approach to determine the efficacy
duration, intervention and of newer agents. Thus, along with outcome, the authors compared the
statistical significance. design, cohort size, participant skin type, duration, intervention, result
measurement, and statistical and clinical significance of several reported
studies. They also examined whether the results of clinical trials for newer
agents based on studies to minimize sources of bias could be accepted,
Save to described next.
My Library
*Adapted from S. Saxena, R. Andersen, and HI Maibach, Pitfalls in clinical trials reveal need for more
tolerable, effective depigmenting agent, J Derm Treatment (Feb. 11, 2015) pp 1-11

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Research | C&T
Table 1. Depigmenting Agent Results
Number Number of Number of

Number of Number of
of Double- Placebo- Trials using
Depigmenting Agent Published Trials not using
blinded controlled Subjective Result
Trials Sunscreen*
Trials trials Measurement
Hydroquinone 22 3 3 2 18
Ascorbic Acid 5 2 3 2 3
Azelaic Acid 1 0 0 1 1
Retinol 7 2 1 2 6
Niacinamide 5 5 4 2 4
Total: 40 12 11 9 32
*Sunscreen usage was not disclosed
Biases Twenty-seven percent of the reviewed trials con-

Sources of bias came from case-control study tained a placebo, although other flaws were present.
designs, which lack placebos, and double-blinded Yun et al. used placebos but the trial was not double-
trials. Additional bias comes from subjective analysis blinded, devaluing statistically significant results.8
of results through patient/investigator analysis.5 In other trials, sunscreens acted as placebos and
As shown in Table 1, 18 of 22 published trials on overall, only eight published trials did not specify
hydroquinone incorporated subjective evaluations to sunscreen use. While sunscreen use does not neces-
document efficacy. However, this method of retrieval sarily attribute to bias, Woodhall et al. showed
is inherently biased, so investigators should have through a placebo-controlled trial that sunscreen
relied on objective assessments such as the Melasma provides a statistically significant reduction of
Area and Severity Index (MASI) score, introduced by hyperpigmentation.9 Using sunscreen in conjunction
Kimbrough-Green et al. The MASI score is calculated with treatment is beneficial to participants suffer-
similar to the scoring system for psoriasis, which ing from hyperpigmentation, but this practice does
assigns a number based on the severity of melasma not improve the investigators’ understanding of a
by evaluating its content, darkness and homogeneity.6 depigmenting agent’s or even sunscreen’s potency.
Other objective assessments can include chromame-
ter measurements and spectroscopy.
Safety and Tolerability
Bias also comes with case-controlled trials Beyond accurate efficacy results, trials should
because investigators and participants know the trials consider safety and tolerability. Since hydroquinone’s
and other areas that are lacking. Castanedo-Cazares toxicity has been questioned, it is not known whether
et al., for example, conducted a double-blind study other agents that inhibit melanogenesis such as
to test the efficacy of niacinamide and desonide ascorbic acid, azelaic acid, retinol and niacinamide,
for hyperpigmentation. They also measured results are toxic.
through colorimetric and clinical evaluations.7 Yet, The majority of the trials referenced lasted 24
even if results include both subjective and objec- weeks, which might not be sufficient time to ascertain
tive analysis, the subjective results still impact the a medical or safety claim, especially taking into
statistical significance and in turn, clinicians will not consideration results were subjective evaluations or
know to what degree objective and subjective results focused on the hyperpigmentation itself, rather than
influence this significance. toxicity. Longer trials would provide more informa-
Placebos are another means to compare efficacy. tion on an agent’s safety. This could help patients
In addition to facilitating double-blind trials, they can decide whether the cost of treatment is worth its risk
highlight other aspects of the disorder; e.g., whether or reward.
hyperpigmentation can improve spontaneously. This Patients having high Fitzpatrick skin types suffer
provides indispensable information for patients, who the most from hyperpigmentation due to their mela-
therefore might not need to risk treatment for curing nocytes being more active.10 And while the referenced
hyperpigmentation. trials did in fact test on skin of color, they did not

test phototypes greater than V. Makino et al., for instance,
performed a double-blind, randomized trial for brighten-
ing formulations,11 and while the results were based on
objective measurements, the study was performed on
Caucasian skin, which is less likely to have issues with
hyperpigmentation.
Unpublished trials followed similar methods concern-
ing design, phototypes and intervention; however, no
statistically significant results were published, nor any
results in general.
Conclusions
Although though there is not sufficient information to
make a conclusion regarding the efficacy of these alterna-
tive products, room for discussion exists. Overall trial
methods support tangible results rather than measuring
efficacy and tolerance. And despite numerous trials, little is
known about the long-term safety and efficacy of depig-
menting agents.
Until a trial is double-blind, long-term, performed on
proper phototypes, placebo-controlled and objectively
measured, one cannot quantify strengths and weaknesses
of these agents with full certainty for hyperpigmentation
treatment.
Intensified action for a safer, more effective formula-
tion than hydroquinone is welcomed. Such a formulation
would ideally be non-irritating, safe over long-term use,
and dermally and systemically effective in comparison
with hydroquinone and placebo products.
References
1. www.pubmedcentral.nih.gov/articlerender.fcgi?artid=2921758&tool=p
mcentrez&rendertype=abstract (Accessed Jul 9, 2014)
2. AM Kligman, A new formula for depigmenting human skin, Arch Derma-
tol, doi:10.1001/archderm.1975.01630130042004 111 (1)40 (1975)
3. www.ncbi.nlm.nih.gov/pubmed/22220462 (Accessed Aug 25, 2014)
4. informahealthcare.com/doi/abs/10.3109/9781420069686.057
(Accessed Jul 17, 2014)
5. KF Schulz and DA Grimes, Case-control studies: Research in reverse,
Lancet, doi:10.1016/S0140-6736(02)07605-5, 359(9304) 431-4 (2002)
6. www.ncbi.nlm.nih.gov/pubmed/19340686 (Accessed Jun 24, 2014)
7. JP Castanedo-Cazares et al, Topical niacinamide 4% and desonide
0.05% for treatment of axillary hyperpigmentation: A randomized,
double-blind, placebo-controlled study, Clin Cosmet Invest Dermatol,
doi:10.2147/CCID.S39246 6:29-36 (2013)
8. IS Yun, H-S Yoo, YO Kim and DK Rah, Improved scar appearance
with combined use of silicone gel and vitamin C for Asian patients: A
comparative case series, Aesthetic Plast Surg, doi:10.1007/s00266-
013-0210-5 37(6) 1176-81 (2013)
9. www.ncbi.nlm.nih.gov/pubmed/19746679 (Accessed Jul 17, 2014)
10. www.ncbi.nlm.nih.gov/pubmed/17354519 (Accessed Jul 16, 2014)
11. www.ncbi.nlm.nih.gov/pubmed/23545928 (Accessed Jul 13, 2014).

Research | C&T
An In vivo Comparison of
Biomimetic vs. Traditional
Skin Moisturization*
Petya Todorova, Peter Grant-Ross and
Slobodanka Tamburic
London College of Fashion, University of the Arts London, UK
Ritva Kurimo
Laurea University of Applied Science, Vantaa, Finland
T
he stratum corneum’s (SC) functional status depends on it being in a
KEY WORDS plasticized state,1 which relies on adequate water-holding and water-
proofing abilities. These abilities will depend on the state of the skin
skin barrier • moisturizers • barrier, which is crucial to human survival. Daily life presents a number
occlusion • humectants • of challenges for this protective layer of the body. These include the use of
biomimetic lipids • simple cleansers,2 UV damage, environmental conditions, aging and skin
hydration • pH diseases. Of these, the effects of aging and the environment were the main
focus for the present study, which was conducted over winter months in a
Nordic country and employed elderly female volunteers.
ABSTRACT Many skin functions decline with age, such as cell regeneration, injury
response, barrier function and sweat and sebum production.3 Dry and flaky
To alleviate skin dryness,
skin is a common condition in elderly people due to a reduced water-
humectants and
binding capacity of the SC, as well as a decline in epidermal regeneration.4
occlusive substances are In fact, the process of renewing the epidermal layer, which would
traditionally used. A third, typically take about 28 days in young adult skin, might increase to 40 to 60
relatively recent approach days with age.5 A significant correlation also has been found between the
is biomimetic, i.e., actives hydration state of the SC and its amino acid content in elderly individuals
with a lamellar structure with dry skin.6 Aged skin is characterized by a decline in water barrier
containing skin-identical repair, which can lead to a loss of the water-soluble natural moisturizing
lipids. The aim of this study factor (NMF) compounds from the surface layers.7
According to Luebberding et al.,8 only some aspects of the skin barrier
was to determine whether
function change with age. Sebum production has been found to decrease
a biomimetic cream significantly with age, but SC hydration either remains unchanged in the
could deliver superior cheeks and hands, or increased in the forehead, neck or forearms. This
moisturization to human information corresponds with some previous studies9, 10 but conflicts with
volunteers, compared with others.11, 12 It also corresponds with the human perception that aged skin
a conventional moisturizer needs more moisturization.4
containing petrolatum and Furthermore, although dry skin has been considered genetically predis-
mineral oil. posed to this state, individuals having different skin types can experience
it due to factors such as climate.13 In studies conducted during summer
and winter months in the U.K., Rogers et al.14 demonstrated a significant
reduction in the levels of SC ceramides and fatty acids in subjects during the
Save to winter. This is why weather is a key consideration in dry skin evaluations.15
My Library Moisturizing products arose from a consumer need to treat and prevent
*This paper was presented at the 28th IFSCC Congress in Paris (Oct 2015).

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Research | C&T
dry skin conditions. The mass market for moistur- These slowly penetrate into the epidermis and rebuild
izers started more than 150 years ago with products the barrier in a natural way by accelerated metabo-
such as petroleum jellya and cold creamb,16 and the lization in the lamellar bodies.21 They also play a
majority of today’s moisturizers are still designed part in the recovery of squamous skin following
around these two traditional approaches; i.e., humec- surfactant damage.22
tants and occlusive agents.17 The skin mechanisms to Another recent study by Pennick et al.23 compared
retain moisture are related to activities of the NMF, the effects of a lamellar cream versus a mineral
lamellar lipid bilayers and the maturation of the oil-containing vehicle in a regression trial employ-
corneodesmosome-bound corneocytes.18 ing expert visual grading. These results showed the
An impaired skin barrier would cause the loss of lamellar cream visibly improved the signs of skin dry-
water-soluble NMF, so the humectancy mechanism ness to a significantly greater extent and maintained a
relies on the application of hygroscopic ingredients better skin condition during the regression phase.
that act in a similar way to NMF. In fact, some Considering the described work, the aim of
humectants used in moisturizing formulations, such the present study was to compare two different
as lactic acid and urea, are components of the skin approaches to skin moisturization in women over
NMF.16 On the other hand, the deposition of oily the age of 60: traditional occlusion vs. biomimetic
materials to the skin surface creates an artificial bar- ingredients. This data could provide insight as to the
rier that restricts evaporation of water from the skin; best approach to re-hydrate aging skin.
i.e. they act as occlusive materials.16
Advanced moisturizers aim to go beyond the Materials and Methods
mechanisms of humectancy and occlusion in order to Materials: An essential factor for the selection
treat the underlying causes of skin dryness,15 e.g., by of skin-identical lipids for a moisturization study
delivering skin lipids, NMF, lipid precursors, peptides is their composition. Studies by Thornfeldt24 and
and amino acids. This biomimetic approach involves Mao-Qiang21 have shown the importance of lipid
the application of multilamellar lipid structures ratios and how topical application of individual lipids
similar to the skin surface lipids to promote the or incomplete mixtures of lipids could interfere with
reconstruction of lamellar structures in the SC and barrier recovery rather than promote it. Two com-
restore skin barrier function.19 mercially available biomimetic active ingredients
Using infrared spectroscopy, Prasch et al.20 have containing approximately 2.5% active content of
studied the mechanisms of strengthening the skin skin-identical lipids were selected for the formulation
lipid film by means of creams. They compared a of test products (see Table 1).
conventional w/o emulsion versus a lamellar cream Active I was a ready-to-use, emulsified lamellar
containing lipids in a structure resembling the lipid system, and Active II was a concentrated lipid paste.
film in the SC. The lamellar cream increased the Both blends claimed to have compositions similar
degree of order of the alkyl chains in the SC in a to skin surface lipids, and both claimed to work by
biomimetic manner, while a standard w/o emulsion forming a protective barrier on the skin and restoring
caused a reduction in the degree of order. This also the missing lipids, thus providing care to dry and sen-
was confirmed by changes measured in skin mois- sitive skin. These were formulated into an emulsion
ture; six hours after application of the two products, vehicle containing glycerin, carbomer, caprylic/capric
the lamellar cream showed a significant increase. triglyceride, preserved water, sodium hydroxide,
Other studies on this topic have suggested disodium EDTA and tocopheryl acetate, stabilized
that while mineral oil causes an immediate partial with an alkyl polyglucoside emulsifier system.
restoration of the skin barrier properties of the SC, Methods: This in vivo study was carried out in
physiological lipid mixtures can have biological two stages: first, a four-hour moisturization study
effects on the metabolism of the living epidermis. on the inner lower legs, and second, a three-week
regression study on the inner lower legs and the
back of hands, in combination with self-assessment
Market Intelligence at baseline and three weeks. The testing equipment
consisted of a corneometerc for both stages and a skin
n The skin care market is not slowing down and is pH meterd for only the second stage.
estimated to reach $121 billion globally in 2016. Short-term protocol: In the first stage of the study,
By 2018, the U.S. skin care market will reach the performance of the two biomimetic prototypes
$10,717.4 million. was evaluated against a non-application site and
a commercial product containing petrolatum and
Source: GCI (GCImagazine.com)
a
Vaseline and b Pond’s Cold Cream, Unilever

mineral oil as moisturizing ingredients. Sixteen Twenty total participants, over the age of 60, were
volunteers from the target age group were recruited provided with color-coded test products to use at
for a four-hour, blind skin hydration trial on the home, with instructions and a basic hand and body
lower legs, using randomized intra-individual, wash to standardize their cleansing routines. The
left-right comparison. subjects traveled to the test center for the corneom-
The study was conducted after a one-week eter and skin pH measurements at baseline, after one
wash-out phase of no moisturizer application on the and two weeks of product application, and at the end
test sites. The better-performing biomimetic proto- of the one-week regression stage.
type was chosen for testing against the commercial Self-assessment: In order to compare the results
product during the second stage of the study. measured instrumentally with the subjects’ impres-
Longer-term protocol: A long-term, two-week sions of the products, the volunteers completed a
(Monday through Friday) study was designed as a self-assessment questionnaire. They were instructed
mini-regression test in which products were applied to note any changes they observed in their skin
twice daily, followed by a
one-week regression phase,
for a total of three weeks. Table 1. Components of Skin Lipids, Active I and Active II
This involved applying the
biomimetic prototype to Skin Lipids Active I Active II
one lower leg (shin) and the Triglycerides Caprylic/Capric Triglyceride Macadamia Triglyceride
back of one hand (dorsal Fatty Acids Palmitic Acid Vegetable Fatty Acids
side), and similarly applying
Cholesterol Phytosterols Soja Bean Sterols
a commercial product to the
other lower leg and hand. Ceramides Ceramide 3 Safflower Ceramides
Phospholipids Phospholipids Soja Bean Phospholipids
c
Corneometer CM825 and d Skin pH
Meter PH905, Courage and Khazaka Squalane Squalane Olive Squalane
Electronic GmbH

Research | C&T
condition during the study. The questionnaire was Figure 1, which shows the results of the Tukey post-
designed to be simple and easily understood, but hoc test and revealed where the significant changes in
also to give information on the subjects’ moisturizing hydration were. For the results shown, A = Active I; B
habits, the performance of the test products, and their = Active II; C = Commercial product; D = No applica-
preference between the two. tion; H0 = Baseline; H1 = 1 hour after application; H2
The data obtained from the two trials were = 2 hr after application; H3 = 3 hr after application;
evaluated using the “R” software package for statisti- and H4 = 4 hr after application.
cal computing and graphics, based on the median Figure 1 shows the two prototypes performed
of three consecutive measurements. The results equally well, and as the B-A segment stretches right
were checked for normality and the methods used across the vertical 95% confidence line, there was
consisted of two-way analysis of variance (ANOVA), no significant difference between the effects they
Student’s t-test and binomial tests. delivered. Both prototypes delivered significantly
higher results compared with the benchmark and
Results and Discussion: the no-application control. The confidence levels for
Short Term prototype A, i.e., the C-A and D-A interactions, were
The aim of this trial was to evaluate and compare slightly higher than those delivered by prototype B,
four-hour effects of the three test products and select i.e., interactions C-B and D-B, which indicates but
a biomimetic prototype for the next stage. First, does not prove better performance.
one-way ANOVA showed no significant differences Interestingly, no significant change was found
in the baseline measurements of the test sites, even in the effects provided by the commercial lotion
though the skin on the lower legs was shown to be compared with the no-application control. This can
quite patchy and gave variations in measurements. be explained by the fact that the occlusive mecha-
Therefore, a two-way ANOVA test with replications nism, which relies on materials, such as petrolatum,
was employed on all the hydration measurements provides better effects over time and with repeated
for the stage one study, to compare the differ- applications.15 On the other hand, the changes in skin
ent test products and check how the two factor hydration delivered by the test products were signifi-
variables—i.e., treatment (test product) and time cant up to two hours after application, compared with
(i.e., after application)—matched up with the variable the baseline values. No other significant differences
hydration response. were found regarding the time after application.
The resulting p values showed a very significant A representation of the variations in skin hydra-
difference (p = 1.274e-07) between the treatments with tion response for the three different treatments and
different test products, and a significant difference (p no-treatment control over the course of the study is
= 0.00861) between the levels of hydration at different presented in Figure 2 on Page 36. The skin hydration
time points. This is visually demonstrated in values for all test products peaked at one hour after
application.
An identical pattern
Figure 1. Tukey HSD test results was observed for the
two biomimetic proto-
types, and the results for
both were much higher
compared with the
occlusive commercial
product. The small drop
in the no-application
control readings at three
hours after application
was analyzed using
two-sample t-test for
hours two to three, and
three to four, to see if
there were any signifi-
cant variations, which
could mean a variation
in test conditions.
The tests showed no
statistical significance.

Research | C&T
As the results of this trial suggest, both Active I sion stage. Although no statistical significance was
and Active II prototypes showed superior perfor- found for the increase between the ends of week two
mance to the commercial product. These findings and week three (the regression phase), results of the
are in accordance with the previously mentioned, baseline vs. post-regression were highly significant
six-hour study by Prasch.20 However, this test is not (p = 0.002229).
conclusive and it is clear that further investigation is On the contrary, the commercial benchmark
warranted to fully study the effects of the products showed no improvement during the course of appli-
in a multiple application trial. The Active I prototype cation, and a statistically significant (p = 0.0008) drop
was chosen for further study due to the slightly in hydration from week two to the end of regression
higher confidence levels (see Figure 1). phase. This decrease was also significant (p = 0.003)
in comparison with the baseline.
Results and Discussion: Skin hydration results of the regression study on
Longer Term the lower legs, shown in Figure 4 on Page 38, reveal
As noted, the second part of this study was similar trends. For this test site, the prototype showed
performed to assess changes in skin hydration and no increase during the first week of application but a
pH levels over time: during two weeks of product statistically significant rise (p = 6.606e-05) during the
application, followed by one week of no product second week. Corresponding to the findings for the
application. The test subjects’ opinions also were hands, hydration in the legs continued to increase
considered and compared with instrumental results. during the regression stage, with no significance
SC hydration: Two-way ANOVA analysis revealed compared to week two but a significant increase over
a significant difference between the two treatments, baseline values (p = 0.001). Also similar to results
both on the hands (p = 1.224e-05) and on the lower in the hands, the benchmark in the legs showed
legs (p = 5.466e-05). No significant difference was a significant decrease during the regression stage
found during product application between weeks compared to week two (p = 0.006) and over the
one and two. These results are shown in Figure 3 on baseline (p = 0.019).
Page 38. The results for different weeks were isolated Overall, the results of both test sites confirmed
and compared using the two-sample paired data superior performance of the biomimetic prototype
t-test. Significant results were marked on the interac- over the standard commercial o/w lotion. This data
tion plot using symbols. corresponds to the findings of Prasch et al.,20 in terms
As Figure 3 shows, after one week, an increase of higher skin hydration obtained from the lamellar-
in hydration values on the hands for the Active I structured cream. A regression test by Pennick et al.23
prototype was observed. However, this showed no employing visual grading also showed positive effects
statistical significance compared with the baseline of lamellar structures.
values. In the second week of application, results Since the reasons behind the increase of skin
increased slightly but continued to rise in the regres- hydration during the regression stage of the prototype
are not fully understood,
further research could ben-
Figure 2. Changes in SC hydration after 4 hr efit from a longer regression
phase, to determine at what
time point the skin would
return to its initial state. A
possible explanation for the
continuous improvement
could refer back to the
work of Mao-Qiang et al,21
which suggests a physi-
ological lipid mixture could
influence the metabolism
of lamellar bodies in the
epidermis and thus improve
the skin barrier function.
Also, the low results
recorded for the benchmark
could be due to the fact
that measurements were
taken three days after the

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Research | C&T
last product application. This suggests that while the skin barrier. This is why pH values of the backs
the biomimetic prototype might be able to deliver of hands and the lower legs were recorded during the
increased skin moisturization up to three days after long term study. Analysis of the data using a 2-way
the last treatment, as observed by Pennick et al.,23 the ANOVA test showed no significant changes in pH
occlusive effects of the benchmark might be limited values for any of the test sites.
to a shorter term efficacy. Self-assessment: The self-assessment question-
Further investigation of these test products is naire revealed volunteers’ moisturizing habits and
required, and with alternative instrumental methods impressions of the two test products; 55% of vol-
such as TEWL and Confocal Raman Spectroscopy unteers considered their skin to be dry, while 35%
to determine changes in the water content of the thought theirs was normal (see Figure 5 on Page 40).
SC and its thickness, as suggested by a study by This data fits with the findings of Luebberding et al.,8
Crowther et al.25 which indicate aging is not always accompanied by
Skin pH: Measurements of the skin surface pH skin dryness. In fact, the questions regarding subjects’
can reveal important information about the state of moisturizing habits showed that 20% of participants
did not moisturize regularly,
Figure 3. Changes in skin hydration on hands and none of them would
typically use a moisturizer
more than once a day.
This shows that although
studies indicate a reduced
water-binding capacity,
decline of the regeneration
of the SC and of the produc-
tion of skin lipids,26 and
significant reduction in skin
hydration with age,11 most
volunteers felt they did not
need to moisturize every
day, with the majority doing
so several times a week.
The effects of the two test
products in delivering skin
moisture and softness were
significant at p < 0.01, per a
2-sample paired data t-test,
for both questions; Figure 6
Figure 4. Changes in skin hydration on legs on Page 40 and Figure 7 on
Page 42 illustrate the results.
The effects of the
Active I prototype were per-
ceived to be better than the
commercial product, which
was in line with instrumen-
tal results. Interestingly, the
negative effects observed for
the benchmark during the
instrumental trial were not
detected by all consumers,
and the product received
scores as high as 8 on a
scale of 1-9. This shows how
equipment can sometimes
identify changes that might
not necessarily be recogniz-
able by the human eye
or touch.

Research | C&T
natural skin barrier can improve skin hydration to a
Figure 5. Self-assessment data of skin greater extent than conventional o/w emulsions based
type (n = 20) on occlusive materials and humectants. In addition,
it suggests that using biomimetic moisturizers is an
effective and longer-lasting method to alleviate dry
skin conditions in women over the age of 60.
In the future, it would be interesting to repeat this
study with older participants (e.g., over 80), since this
group tends to suffer from the unpleasant conse-
quences of very dry skin and could greatly benefit
from effective and long-lasting moisturization.
References
1. GK Menon and L Norlen, Stratum corneum ceramides and their
role in skin barrier function, in J Leyden and AV Rawlings, eds,
Skin Moisturization, Marcel Dekker, New York (2002)
2. TG Polefka, Surfactant interactions with skin, in U Zoller and
Figure 6. Self-assessment of skin G Broze, eds, Handbook of Detergents. Part A: Properties,
Marcel Dekker, New York (1999)
moisturization 3. B Gilchrest and J Krutmann, Skin Aging, Springer, Berlin (2006)
4. E Proksch, Dryness in chronologically and photo-aged skin,
in M Loden and HI Maibach, eds, Dry Skin and Moisturizers:
Chemistry and Function 2nd edn, CRC Press, Boca Raton
(2006)
5. AM Kligman, Perspectives and problems in cutaneous gerontol-
ogy, J Inves Derm 73(1) 39-46 (1979)
6. I Horii, Y Nakayama, M Obata and H Tagami, Stratum corneum
hydration and amino acid content in xerotic skin, Brit J Derm
121 587–592 (1989)
7. EM Zettersten, R Ghadially, KR Feingold, D Crumrine and PM
Elias, Optimal ratios of topical stratum corneum lipids improve
barrier recovery in chronologically aged skin, J Amer Acad Derm
37 403-408 (1997)
8. S Luebberding, N Krueger and M Kerscher, Age-related changes
in skin barrier function–Quantitative evaluation of 150 female
subjects, Int J Cos Sci 35 183–190 (2013)
9. V Agarwal, M Godfrey, S Long, D Whitby, S Barton and A
Desnos, Variability in the physical properties of the stratum
corneum–Influences of chronological age and season, Int J Cos
Further, apart from delivering superior moisturiza- Sci 29(3) 219 (2007)
tion, the biomimetic prototypes were designed to 10. KP Wilhelm, AB Cua and HI Maibach, Skin aging. Effect on tran-
sepidermal water loss, stratum corneum hydration, skin surface
provide a better texture and improved skin feel than pH and casual sebum content, Arch Derm 127(12) 1806-1809
the products based on the occlusive mechanism. The (1991)
opinion of the volunteers on this matter is demon- 11. IL Shlivko et al, Complex assessment of age-specific morpho-
functional features of skin of different anatomic localizations, Skin
strated in Figure 8 on Page 42. This data was analyzed
Res and Tech 19 85–92 (2013)
using a two-sided binomial test, and the 65% of 12. P Thune, T Nilsen, IK Hanstad, T Gustavsen and H Lövig-Dahl,
individuals preferring the texture of the biomimetic The water barrier function of the skin in relation to the water
prototype did so at a significant 99% confidence level. content of stratum corneum, pH and skin lipids. The effect
of alkaline soap and syndet on dry skin in elderly, non-atopic
On a whole, the self-assessment questionnaire patients, Acta Dermato-Venereologica 68 277–283 (1988)
revealed that the Active I prototype was the preferred 13. V Couturaud, Biophysical characteristics of the skin in relation
option to the commercial product in delivering to race, sex, age and site, in AO Barel, M Paye and HI Maibach,
eds, Handbook of Cosmetic Science and Technology 3rd edn,
benefits to the skin and for its sensory properties. This Informa Healthcare, London (2009)
reflects the outcomes of the four-hour instrumental 14. J Rogers, CR Harding, A Mayo, J Banks and AV Rawlings,
trial and three-week regression study, and compli- Stratum corneum lipids: The effect of aging and the seasons,
ments other instrumental studies20-22 and a visual Arch Derm Res 288 765-770 (1996)
15. G Nole, Clinical testing of moisturizers, in J Leyden and AV
grading study,23 showing that the measured effects can
Rawlings, eds, Skin Moisturization, Marcel Decker, New York
also be identified by the consumers. (2002)
16. AW Johnson, The skin moisturizer marketplace, in J Leyden and
Conclusion AV Rawlings, eds, Skin Moisturization, Marcel Dekker, New York
(2002)
The present study demonstrates that providing the
skin with lipids identical to those that make up the

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Research | C&T
Figure 7. Self-assessment of skin softness
Figure 8. Preference for test product textures
17. B Chavan, G Pennick, B Summers and AV Rawlings, Effect of an

amphiphilic self-assembled lipid lamellar phase on the relief of dry skin,
Stratum Corneum VII conference presentation (2012)
18. AV Rawlings and PJ Matts, Stratum corneum moisturization at the
molecular level: An update in relation to the dry skin cycle, J Inves Derm
124 1099–1102 (2005)
19. JK Jung, YH Ahn, SM Bae and JG Hwang, Study on the bio-mimic
liquid crystal emulsion for skin barrier, IFSCC conference presentation,
Amsterdam (2007)
20. T Prasch, G Knübel, K Schmidt-Fonk, S Ortanderl, S Nieveler and
T Förster, Infrared spectroscopy of the skin: Influencing the stratum
corneum with cosmetic products, Int J Cos Sci 22 371–383 (2000)
21. M Mao-Qiang, BE Brown, S Wu-Pong, KR Feingold and PM Elias,
Exogenous nonphysiologic versus physiologic lipids. Divergent mecha-
nisms for correction of permeability barrier dysfunction, Arch Derm 131
809-816 (1995)
22. G Imokawa, S Akasaki, Y Minematsu and M Kawai, Importance of
intercellular lipids in water-retention properties of the stratum corneum,
Induction 281 45-51 (1989)
23. G Pennick, B Chavan, B Summers and AV Rawlings, The effect of an
amphiphilic self-assembled lipid lamellar phase on the relief of dry skin,
Int J Cos Sci 34 567-574 (2012)
24. C Thornfeldt, Critical and optimal molar ratios of key lipids, in M Loden
and HI Maibach, eds, Dry Skin and Moisturizers: Chemistry and Func-
tion 2nd edn, CRC Press, Boca Raton (2000)
25. JM Crowther et al, Measuring the effects of topical moisturizers on
changes in stratum corneum thickness, water gradients and hydration
in vivo, Brit J Derm 159 567–577 (2008)
26. E Proksch, Dryness in Chronological and Photo-Aged Skin, CRC Press,
Boca Raton (2006)

Testing | C&T
Yield Stress Measurements

for Personal Care, Part I:
Definitions and Basics
Jeffrey Martin, Ph.D.
Johnson & Johnson
Consumer and Personal Products Worldwide
Skillman, NJ USA
F
ormulators often suspend insoluble ingredients such as scrubbing
KEY WORDS beads, pearlizer crystals, oils, actives, etc., in formulations. In addition,
creamy, lotion-like and thick or substantial textures often are desired.
yield stress • deformation • Both of these characteristics, i.e., the suspension capability and a creamy
observation • timescale • texture, are realized by a formulation’s yield stress.
Deborah number • putty • Yield stress often is confused with high viscosity, but increased viscosity
Weissenberg number • only causes longer settling times, it does not impart true suspension. In rela-
solid-like • liquid-like • tion, the aim of this article is threefold: to properly define and differentiate
solid-liquid balance • yield stress from high viscosity; to develop a method and provide calcula-
frequency sweep • tions for assessing whether a sample has a yield stress; and to illustrate how
to determine the amount of yield needed for a given application. In part
suspension • robustness
two of this series, several popular methods to measure yield stress will be
explored and compared and contrasted in terms of relevance, exactness and
robustness.
ABSTRACT
The aim of this article Defining Yield Stress
series is to properly define Since the earliest days of measuring yield stress, scientists and engineers
have debated what method would provide the most exact and relevant
and differentiate yield
values. Many methods exist and different measurements performed on the
stress from high viscosity, same materials often report different values. In fact, for some materials,
as well as develop a identical measurements performed at different deformation rates often
method for assessing provide different yield stress values. Considering intrinsic properties such
whether a sample has a as temperature, mass or density should be independent of the measure-
yield stress. In addition, ment method, this begs the question of whether or not yield stress is a true
it will illustrate how to intrinsic material property.1-4
determine the amount of This debate is complicated by the fact that there is no universally
accepted definition for the yield stress. One common definition is “the
yield needed for a given
stress above which a material flows.” However, every material that can be
application. measured appears to exhibit flow under certain conditions. For example,
long plastic pipes and rock slabs often sag irreversibly over time, indicating
irreversible flow or “creep.”5 The pitch drop experiment, which is in the
Guinness Book of World Records as the longest continuously running labora-
tory experiment, is another example of this phenomenon.6
Save to
Although these materials are experiencing stresses below their yield
My Library
stresses, they are still flowing—albeit slowly. It turns out these solids are
undergoing irreversible flow with extremely large creep viscosities; approxi-

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Testing | C&T
mately 230 billion centipoise, in the case of pitch.7 So A Deborah number, De, is defined as the ratio
are the pitch and rock slabs really flowing or are they of a characteristic timescale of a material, such as a
solid, as everyday experiences would indicate? And is relaxation time (τ), to the time of observation. This is
creep considered flow? If so, does this invalidate the expressed as:
“true” yield stress position? Two valid arguments can
τ
be made for either case, i.e., no yield stress versus a De
≡ Eq. 1
tobv
true yield stress, but the crux of the dispute is how to
define flow and how long to look for it. On the other hand, the Weissenberg number, Wi, is
defined as the ratio of a characteristic timescale of a
Deformation, Observation and material to the rate of deformation, i.e.:
Characteristic Timescales
Here, it is useful to highlight three distinct times- Wi ≡τ
γ •
Eq. 2
cales: the timescale of deformation, the timescale of
observation, and the characteristic timescale of a mate- where γ• is the shear rate.
rial. The timescale of deformation is not how long a To illustrate these concepts, consider Silly Puttya.
deformation is imposed. Rather, it should be thought As is generally known, it behaves more like a solid
of as a characteristic timescale of the flow; like a shear under fast deformations, e.g., it will bounce on the
floor and it behaves more like a liquid under slow
deformations, flowing into a puddle if left on a table.
Putty, for example, How can one material exhibit both solid- and liquid-
like behavior that is so different? This is explained
can exhibit different through the Weissenberg and Deborah numbers.
While the meaning of observation time and shear
behaviors depending rate for these equations should be evident, relaxation
time requires further explanation. In the puttya
on the rate of applied example, the characteristic relaxation time is the time
it takes for the polymer network to relax the stress
deformation. caused from an imposed deformation. If the putty is
deformed at a faster rate than its relaxation time, it
will not be able to dissipate the stress, so the excess
rate, for example. The timescale of observation is the energy will be stored. This is the case of Wi > 1 and
time over which the sample response is measured and the putty will behave more solid-like, storing more
the characteristic timescale of a material is roughly energy than what is dissipated and bouncing on the
how long it takes for said material to relax after it is floor like a piece of solid rubber.
deformed. If the putty is deformed at a slower rate than its
For example, a rubber band will snap back to relaxation time or Wi < 1, it can dissipate more stress
its original shape quickly after it is deformed; on than what is stored and will behave more liquid-like,
the other hand, the foam topper on a mattress may flowing into a puddle. Thus, the putty can exhibit
take several seconds to even minutes to return to its different behaviors depending on the rate of applied
initial shape after it is deformed. Thus, a rubber band deformation and the Weissenberg number tells us
and mattress foam have very different characteristic where the material is on the spectrum of solid- to
timescales. liquid-like behavior, for a given deformation rate.
The Deborah number requires a different thought
process. While shear rate was used for calculating
the Weissenberg number, here it is not. The Deborah
number does not include information about the
Market Intelligence type of flow, it only includes information about the
observation time and characteristic timescale of the
n Smell and touch are but two facets of a
material. Regardless of the type of flow, the Deborah
formulation. Indeed, the other sensory benefits a
number illustrates the importance of the experi-
product can deliver provide the brand with another
mental observation time with respect to the intrinsic
opportunity to stand out from its competition.
timescale of the material being measured.
Consumers not only enjoy how products feel, but
As an illustration, imagine grabbing onto the
also the entire experience products create.
puttya and quickly pulling it apart a few inches, while
Source: GCI (GCImagazine.com)
a
Silly Putty is a trademark of Crayola, LLC.

constantly observing the feeling of its resistance. The relax-
ation time of the puttya is on the order of 0.1 sec to 0.01
sec; this is the time it takes the putty to relieve all of the
initial stress imposed by pulling it apart. Thus, at observa-
tion times shorter than the relaxation time (De > 1), the
putty behaves more like a solid because the material is not
able to relax the stresses imposed by the initial deforma-
tion and more energy is stored than released. In this case,
the putty would pull back like a rubber band, acting more
solid-like and thus be deemed to have a yield stress. How-
ever, at observation times longer than the relaxation time
(De < 1), all of the initial stress would have been relaxed;
the putty would begin to flow and sag and therefore
deemed to not have a yield stress.
Every “solid,” from glass in windows to steel in cars, has
its own distinct relaxation time. It may not be as fast as the
puttya, but it is finite. The relaxation time for window glass
at room temperature is estimated to be longer than 1 x 1022
years, i.e., a one with twenty-two zeros after it, which is
one million million times longer than the estimated age of
our universe.8 Does this mean everything flows eventually
and there is no true yield stress?
A particularly obstinate measurer could define the
yield stress as strictly as possible, where one measures zero
irreversible deformation over an infinite amount of time
for all applied stresses below the yield stress. This case
corresponds to De = 0, where a measurement is con-
ducted over an infinite amount of time. Such infinite time
measurements are obviously not practical and more suited
to the realm of theology.9-11
Interestingly, the Deborah number is named after
the prophet Deborah, who stated in verse 5:5 of the
Biblical Book of Judges, “the mountains flowed before the
Lord.” There is debate as to the exact translation of this
passage,10, 11 but it is thought that Marcus Reiner, who
defined the Deborah number in 1928 alongside of Eugene
Bingham, intended to imply something as seemingly solid
and immovable as a mountain range would flow over the
infinite timescale of a “supreme being” observer. Further-
more, the motto for the Society of Rheology, attributed to
the philosopher Heraclitus, is “πάντα ῥεῖ,” which translates
to “everything flows.”
Since the aim of this article series is not philosophical
or theological in nature, yield stress will instead refer to
G.W. Scott Blair’s 1933 definition as “the stress below,
which no flow can be observed under the conditions of
experimentation,” (emphasis is this author’s).12 Such a
definition does not restrict the yield stress to being either
a useful engineering concept or a true intrinsic property;
both interpretations are possible, depending on how
long the observer is willing to wait and how sensitive his/
her instruments are. This definition for the yield stress
effectively avoids debate and relieves researchers from
performing infinite-time measurements to determine a
yield stress.

Testing | C&T
Long Timescales and toothpaste. However, it can sometimes be difficult to
differentiate when a formulation has a yield stress,
Suspension or just appears stable over long times due to a high
As discussed, timescales are important in the viscosity. The key factor, which determines whether a
context of the yield stress. In fact, two distinct types material has a yield stress, is the solid-liquid balance.
of yield stresses depend on the relevant timescale: Solid-liquid balance: The solid-liquid balance is
static and dynamic. The static yield stress is defined a measure of the amount of solid-like and liquid-like
as the stress required to initiate flow from rest and character a material exhibits. Since all materials are
the dynamic yield stress is defined as the minimum viscoelastic to some degree, they will have varying
stress required to sustain flow from an already degrees of both solid-like and liquid-like characters.
flowing state.13, 14 Static yield stresses are relevant for For example, mineral oil will exhibit a large liquid-
long-time processes such as sedimentation, whereas like character and low solid-like character, and a
dynamic yield stresses are relevant in dynamic rubber band will be the opposite. This section dem-
processes such as pumping. The static yield stress onstrates how to measure the solid-liquid balance,
is often, but not always, larger than the dynamic then how to use this value to determine whether a
yield stress. sample of interest possesses a yield stress under the
Formulators and product developers often are conditions of interest.
concerned with the yield stress in the context of The solid-liquid balance is a concept commonly
long-timescale processes, e.g., suspending ingredients encountered in the field of rheology and is often
including insoluble benefit agents, beads, pearlizers referred to as tan(δ), the tangent of the phase lag δ
and sometimes air bubbles, for visual appeal. Before between the input and output strain/stress waves of
deciding how to measure a yield stress for this con- an oscillatory experiment conducted on a rheometer.5
text, however, the timescale of interest in the context Another definition incorporates the elastic and
of ingredient suspension must be determined. viscous moduli:
The force driving sedimentation or creaming is
the buoyancy force, caused by the density difference tan(δ) = Gʹʹ
⁄
Eq. 3
between the suspended agent and surrounding fluid Gʹ
matrix. This buoyancy force is driven by gravity, and The elastic modulus Gʹ can be thought of as the
is opposed by the yield stress (if present). Since the amount of energy a material can store (solid-like)
timescale of deformation imposed by the density and the viscous modulus Gʹʹ can be thought of as
difference is driven by gravity, this force acts over an the amount of energy lost due to viscous dissipation
infinitely long timescale—i.e., gravity is a constantly (liquid-like). The solid-liquid balance can vary from
applied force. So in this case, the timescale of interest zero in a perfect solid, to infinity in a perfect liquid,
is infinite. with the transition point from solid-dominated to liq-
In order to stay more practical, the timescale uid-dominated behavior occurring at a value of one:
of interest can be trimmed down to the shelf-life where Gʹʹ = Gʹ. Thus, if Gʹ > Gʹʹ or tan(δ) < 1, the
of a typical product, generally round three years. material exhibits more solid-like character and has
However, the only way to absolutely ensure stability a yield stress, since the yield point is the transition
for three years is to conduct a stability experiment from more solid-like to more liquid-like behavior.5
for three full years, since there is no measurement to However, tan(δ) does not have just one value for
speed up time. Yet, it is still impractical to wait three a given material, it is a time-dependent quantity,
years for guaranteed stability results, so rheology meaning it varies depending on the timescale of
allows us to anticipate longtime behavior through a deformation. For example, the earlier puttya example
few simple experiments. These experiments, outlined showed the material behaved more like a solid under
next, will determine whether a material has a yield shorter deformations, bouncing on the floor, but
stress at a timescale of interest. more like a liquid under longer time deformations,
flowing into a puddle if left on a table. It can therefore
Determining Yield Stress be stated that the putty has a tan(δ) < 1 (solid-like)
Some formulations typically do not have yield under faster deformation rates (shorter times) and
stresses; for example, simple cleansers and other > 1 (liquid-like) under slower deformation rates
systems, where the microstructure is solely surfactant (longer times).
micelles, with or without micellar thickeners. On the Frequency sweep test: In the case of suspending
other hand, products with microstructures consist- ingredients, formulators are interested in longer
ing of networks such as colloidal gels, associative timescales and the behavior of tan(δ) at these long
polymers, etc., generally exhibit yield stress behav- timescales. To determine the behavior of the solid-
ior; examples include creams, lotions, scrubs and liquid balance over varying timescales, a frequency

sweep test must be performed. A frequency sweep ously not feasible as the experiment itself would take
is an oscillatory test performed in a rheometer by three years.
applying a sinusoidal deformation at a fixed ampli- Unfortunately, there are no shortcuts here; a
tude while varying the frequency of oscillation. In rheometer is not a time machine. However, one can
a frequency sweep, the frequency of oscillation is take limiting values of tan(δ) since frequencies tend-
equivalent to the reciprocal of the time of observa- ing toward zero are useful estimations of long-time
tion. This can be expressed as: behavior. Typically, a frequency sweep is conducted
1 from 100 to 0.1 or 0.01 rad/sec; and if tan(δ) < 1 at
ω=
Eq. 4 low frequencies tending toward zero, one can say
tobv
with confidence the material likely has a yield stress
where ω is the frequency of oscillation. It follows that at longer times, even though only a timescale of
the Deborah number for oscillatory flows is: (0.01 rad/sec)-1 or 100 sec is measured. It is important
to note each frequency sweep must be conducted in
De = τω Eq. 5 the linear viscoelastic regime, meaning the applied
strain or stress does not appreciably disturb the
It is important to note for steady, not oscillatory microstructure.
shearing flows, the inverse of the shear rate is not Now that yield stress has been properly defined,
equivalent to the timescale of observation.15, 16 In and a determination made as to whether the mate-
steady shearing flows, the timescale of observation rial has a yield stress at the timescale of interest, the
is simply how long the sample is measured, which amount of yield needed for a given application can be
is independent of the shear rate. Since the longest determined.
timescale of interest is the shelf-life of the product—
again, typically around three years—to guarantee How Much Yield Stress?
absolute stability, one would need to measure a tan(δ) When designing a formulation to suspend an
< 1 at a frequency of roughly 1 x 10-8 rad/sec, which is ingredient, the question arises, “How much yield
the inverse of three years in seconds. This is obvi- is necessary?” To answer this, one must look at the

Testing | C&T
forces involved. The suspended ingredients usually have
densities differing significantly from the suspending
medium, which most commonly is water. Thus, there is
a driving force for the particles to rise or settle, depend-
ing on whether their density is greater or less than the
suspending medium—i.e., the buoyancy force. This force
is exerted by the particle on the fluid and is given by the
particle volume multiplied by its buoyancy. For a spherical
particle, this force is calculated as:17
Fp=
4 Eq.
πR3 g∆ρ 6
3
where R is the particle radius, g is the acceleration due to
gravity, and ∆ρ is the absolute value of the density differ-
ence between the particle and the surrounding medium.
The fluid yield stress also exerts a force on the particle,
which for a spherical particle is given by:17
Ff = 2πR2σy Eq. 7
where σy is the yield stress. In order to suspend the

particle, the force of the yield stress must be larger than the
force exerted by the particle. Thus, one can define a ratio of
the force exerted by the yield stress to the force exerted by
the particle as:17, 18
Ff 1.5 σy
=
Y Eq.
= 8
Fp Rg∆ρ
Note Equation 8, as written, is for spherical particles; Y

can be derived for other particle shapes as well.
If the fluid yield stress is larger than the stress exerted
by the particle rising or falling (Y > 1), the particle will
be suspended. If the stress exerted by the particle is larger
than the yield stress (Y < 1), the particle will overcome the
yield stress and begin to move. However, the value of Y at
which particles are suspended, denoted as Ycrit, is found
experimentally to be considerably less than one for various
reasons, which are discussed elsewhere.18
Experimental and theoretical values of Ycrit have been
shown to range from 0.05–0.6, depending on particle
shape, experimental conditions and type of yield stress
fluid. In fact, for identical particles, different values of
Ycrit were reported for different types of yield stress fluids,
namely an associative polymer (cellulose fiber, e.g., xan-
than gum) and a colloidal gel (carbomer).18 Since the value
of Ycrit for a given particle and yield stress fluid cannot be
known a priori, a value of Ycrit ≥ 1 can be taken as a safe
guideline when formulating.
Note with changing temperature, the yield stress and
therefore Ycrit also will change. To ensure stability at an
elevated temperature, the yield stress and Y must therefore
be measured at said temperature. It is important to note
yield stress measurements at elevated and room tempera-

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Testing | C&T
tures cannot account for chemical degradation, which sometimes occurs over
time and leads to decreased yield stress values upon stability testing.
It also should be noted Equation 8 is not valid if the size of the particle is com-
parable to the size of the network mesh of the yield stress fluid. As an example, the
network mesh size of a carbomer gel would be the size of the swollen carbomer
domains (on the order of a few hundred micrometers) and the mesh size of an
associative polymer network would be the average distance between associations.
For particles or insoluble actives that are very small, i.e., on the order of the
network mesh size, these can settle through the spaces in between the yield stress
fluid network, without having to overcome the yield stress.18
Example 1:
Jojoba Ester Beads
To illustrate the above concepts, consider whether a formulation having a
yield stress of 1.7 Pa could suspend beads made of jojoba esters having a diameter
range of 250–400 μm and a specific gravity of 0.907. To solve for the yield stress
necessary to suspend the particle, Equation 8 is rearranged for σy and Y is set to
one as the stability criterion:
Eq. 9
Rg∆ρ (2 × 10-4 m)(9.8 m/sec2 )(997-907 kg/m3)

σy = = = 0.11 Pa
1.5 1.5
Note the density of water at 25°C is 997 kg/m3 and a quick check of unit consis-
tency shows the units above are correct:
Eq. 10
N kg • m kg
Pa = = =
m2 m2 • sec2 m • sec2
A diameter of 400 μm was used in Equation 9 as a worst-case scenario; larger

particles have a larger sedimentation force (see Equation 6). With a yield stress
of 1.7 Pa, Equation 8 can be used to calculate a value of Y = 15. This is well above
the safe value of Y = 1 and the formulation should be able to suspend the beads,
barring any chemical degradation over time.
Example 2: Air Bubbles

As another exercise, one can calculate the size of air bubbles that can be sus-
pended for a given yield stress. Rearranging Equation 8 for R and setting Y = 1:
Eq. 11
1.5 σy 1.5(1.7 Pa)

R= = = 260 μm
g∆ρ (9.8 m/sec2)(997-1.18 kg/m3 )
Thus, the formula will suspend air bubbles with a diameter of about 520 μm
(0.52 mm) or less; bubbles larger than this size will rise.
Robustness
It is important to note the yield stress value calculated from Equation 9 is
the minimum yield value for infinitely long deformation timescales, and that

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Testing | C&T
the values measured are always time-dependent For example, one may measure a yield stress at
because measurements are conducted over a finite 0.1 rad/sec that is sufficient to suspend the jojoba
timescale. This is important in the context of formula
ester particles at long times when the formulation is
robustness. at rest. However, the product may experience vibra-
tion and other deformation
at faster timescales during
Figure 1. A frequency sweep at 5% strain for a cleanser containing transport and handling.
wormlike micelles and an acrylates copolymer
One could check the
stability of the product
under faster deformation
rates by performing yield
stress measurements at
these faster rates, which
can be time-consuming. A
more qualitative sense of
stability can be gained by
examining the behavior of
the solid/liquid balance in
the frequency sweep.
Remember, tan(δ) must
be < 1 for the sample to
possess a yield stress, so
if tan(δ) is close to one or
exceeds one at moderate
frequencies, yield stress
measurements should

Testing | C&T
be performed at faster deformation rates to ensure given. Taken together, these considerations provide
stability under these conditions. For example, the the framework for a protocol to prepare and evaluate
frequency sweep of a cleanser containing wormlike samples as follows:
micelles and an acrylates copolymer is shown in 1. Determine type of yield stress relevant for
Figure 1. The yield stress measured by an amplitude application (static vs. dynamic).
sweep at 0.1 rad/sec was 1.7 Pa—more than sufficient 2. Determine if sample has a yield stress at a
to suspend the jojoba beads as calculated above. timescale of interest:
However, at frequencies between about 0.7 rad/sec a. Long timescales: tan(δ) < 1 as ω→0,
to 60 rad/sec, tan(δ) is > 1, which means the sample b. Shorter timescales: tan(δ) < 1 at the times-
does not have a yield stress under these conditions. cale of interest.
Thus, if the sample experiences deformations on a 3. If the sample has a yield stress, determine how
timescale between 0.02 sec to 1.4 sec, i.e., the inverse much yield is needed (see Eq. 8); and
of the frequency range, the beads would settle. Any 4. Measure yield stress.
deformations faster than 0.02 sec or slower than As noted, in part two of this series, popular
1.4 sec need to be large enough in amplitude to methods to measure yield stress will be explored,
overcome the yield stress at that timescale for the then compared and contrasted in terms of relevance,
beads to settle. Thus, this product may appear stable exactness and robustness.
under quiescent stability conditions, but may not be
robust under more rigorous conditions. Acknowledgements: The author would like to acknowledge Thomas Hu
for input, and Don Harper, Tobias Fütterer, Davide Miksa, and Michael
Fevola for general feedback and proofreading.
Conclusion
This article has robustly defined yield stress and
References
outlined a process to determine if a sample of interest
1. HA Barnes and K Walters, The yield stress myth, Rheologica
possesses a yield stress at a timescale of interest. It Acta 24 323–326 (1985)
also has illustrated how to calculate the amount of 2. HA Barnes, The ‘yield stress myth?’ paper—21 years on,
yield needed to suspend an ingredient of interest; Applied Rheology 17 (2007)
examples of jojoba ester beads and air bubbles were 3. HA Barnes, The yield stress—a review or ‘panta rei’—everything
flows?, J Non-Newtonian Fluid Mechanics 81 (1999)
4. G Astarita, Letter to the editor: The engineering reality of the
yield stress, J Rheology 34 275–277 (1990)
5. CW Macosko, Rheology: Principles, Measurements and Appli-
cations, VCH Publishers, New York (1994)
6. http://smp.uq.edu.au/content/pitch-drop-experiment (Accessed
Aug 19, 2015)
7. R Edgeworth, BJ Dalton and T Parnell, The pitch drop experi-
ment, Eur J Physics 5 (1984)
8. ED Zanotto and PK Gupta, Do cathedral glasses flow?—Addi-
tional remarks, Amer J Physics 67 260–262 (1999)
9. M Reiner, The Deborah number, Physics Today 17 62 (1964)
10. MM Denn, Just what did Deborah say, Rheology Bulletin 80
(2011)
11. M Boehm, Why did the mountains do anything at all, Rheology
Bulletin 81 (2012)
12. GWS Blair, On the nature of “yield-value,’’ J Applied Physics 4
(1933)
13. DCH Cheng, Yield Stress—A time-dependent property and how
to measure it, Rheologica Acta 25 542–554 (1986)
14. A Fall, J Paredes and D Bonn, Yielding and shear banding in soft
glassy materials, Phys Rev Letters 105 (2010)
15. AB Metzner, JL White and MM Denn, Constitutive equations for
viscoelastic fluids for short deformation periods and for rapidly
changing flows: Significance of the Deborah number, AIChE J
(12) 863–866 (1966)
16. J Dealy, Weissenberg and Deborah numbers—Their definition
and use, Rheology Bulletin 79 14–18 (2010)
17. AN Beris, JA Tsamopoulos, RC Armstrong and RA Brown,
Creeping motion of a sphere through a Bingham plastic, J Fluid
Mechanics (158) 219-244 (1985)
18. H Emady, M Caggioni and PT Spicer, Colloidal microstructure
effects on particle sedimentation in yield stress fluids, J Rheology
57 (2013)

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Formulating | C&T
Suppliers REferenced
AAK Induchem AG Silab
SE 374 82 Karlshamn Sweden Volketswil Switzerland 19108 Brive France
Tel: 46-454-82000 Tel: 41-44-908-4333 Tel: 33-5-55-84-58-40
Fax: 46-454-82885 Fax: 41-44-908-4330 Fax: 33-5-55-84-95-64
lipid@aak.com salesusa@induchem.com silab@silab.fr
www.aakpersonalcare.com www.induchem.com www.silab.fr
BASF Corporation Innospec Sterling Technology

Florham Park, NJ USA Ellesmere Port Brookings, SD USA
Tel: 1-800-880-5768 United Kingdom Tel: 1-605-692-0456
Fax: 1-973-245-6764 Tel: 1-877-700-0302, angela.walter@
beautycare-na@basf.com 0151-355-3611 sterlingtechnology.com
personal-care.basf.com Fax: 0151 356 2349 www.sterlingtechnology.com
emea-pc@innospecinc.com
BASF SE www.innospecinc.com Sytheon Ltd.
Ludwigshafen Germany Boonton, NJ USA
Tel: 1-800-531-0815, Kobo Products Inc. Tel: 1-973-988-1075
49-00800-2273-4444 South Plainfield, NJ USA Fax: 1-973-909-9922
Fax: 49-211-7981-9727 Tel: 1-908-757-0033 info@sytheonltd.com
beautycare-eu@basf.com Fax: 1-908-757-0905 www.sytheonltd.com
www.beautycare.basf.com/ info@koboproductsinc.com
www.koboproducts.com TRI-K Industries
Biosil Technologies Inc. Denville, NJ USA
Allendale, NJ USA Lonza Personal Care Tel: 1-973-298-8850
Tel: 1-201-825-8800 South Plainfield, NJ USA Fax: 1-973-298-8940
Fax: 1-201-825-8810 Tel: 1-908-561-5200 info@tri-k.com
bioinfo@biosiltech.com Fax: 1-618-258-6808 www.tri-k.com
www.biosiltech.com lonzapc.arch@lonza.com
www.lonza.com
Centerchem Inc.
Norwalk, CT USA Lubrizol Advanced Materials,
Tel: 1-203-822-9800 Inc.
Fax: 1-203-822-9820 Brecksville, OH USA
cosmetics@centerchem.com Tel: 1-800-379-5389,
www.centerchem.com 1-216-447-5000
Fax: 1-216-447-5740
Croda personalcare@lubrizol.com
Edison, NJ USA www.lubrizol.com/personalcare
Tel: 1-800-526-5294,
1-732-417-0800 Lucas Meyer Cosmetics
Fax: 1-732-417-0804 Quebec, QC Canada
rosalind.brooks@croda.com Tel: 1-877-886-4739,
www.crodapersonalcare.com 1-418-653-6888
Fax: 1-418-653-6005
Croda Europe Ltd. info@lucasmeyercosmetics.com
Goole United Kingdom www.lucasmeyercosmetics.com
Tel: 44-1405-860551
Fax: 44-1405-861767 Mibelle Biochemistry
pc-europe@croda.com Buchs Switzerland
www.croda.com/europe/pc Tel: 41-62-836-17-31
Fax: 41-62-836-14-05
Custom Ingredients info@mibellebiochemistry.com
Chester, SC USA www.mibellebiochemistry.com
Tel: 1-803-377-1213
Fax: 1-803-581-5802 Nikko Chemicals Co., Ltd.
sales@custoblend.com Tokyo Japan
www.custoblend.com Tel: 81-3-3661-1677
Fax: 81-3-5614-8250
Deveraux Specialties, LLC inter@nikkol.co.jp
Sylmar, CA USA www.nikkol.co.jp
Tel: 1-818-837-3700
Fax: 1-818-837-3778 Seatons (Croda Group)
info@deverauxspecialties.com East Yorkshire United Kingdom
www.deverauxspecialties.com Tel: 44-1405-860551
Fax: 44-1405-861767
DSM Nutritional Products pc@croda.com/seatons
Parsippany, NJ USA www.croda.com/seatons
Tel: 1-800-526-0189
webshop.dnpna@dsm.com Sederma
www.dsmnutritionalproducts.com 78612 Le Perray-en-Yvelines
Cedex France
Floratech Tel: 33-0-1-34-84-10-10
Chandler, AZ USA Fax: 33-0-1-34-84-11-30
Tel: 1-480-545-7000 sederma@sederma.fr
Fax: 1-480-892-3000 www.sederma.com
sales@floratech.com
www.floratech.com

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Advertiser Index | C&T
A&E Connock Ltd. Courage & Khazaka GmbH Lucas Meyer Cosmetics
C2 4 5
sales@connock.com info@courage-khazaka.de info@lucasmeyercosmetics.com
www.connock.co.uk www.courage-khazaka.de www.lucasmeyercosmetics.com
(p. 33) (p. 60, 62)
AMA Laboratories, Inc.
19
www.amalabs.com Croda, Inc. Naturex SA
7 21
(p. 25) marketing-usa@croda.com naturex@naturex.com
www.crodausa.com www.naturex.com
Angus Chemical Company p. 60, 62)
51
info@angus.com Nikko Chemicals Co. Ltd.
39
www.angus.com Dr. Straetmans Chem. Prod. www.nikkol.co.jp
25
GmbH (p. 60, 62)
Arista Industries, Inc. info@dr-straetmans.de
47
info@aristaindustries.com www.dr-straetmans.de Pilot Chemical Co.
54
www.aristaindustries.com (p. 10) info@pilotchemical.com
www.pilotchemical.com
BASF Dupont Tate & Lyle BioProducts
31 22
yvonne.specht@basf.com www.duponttateandlyle.com Reed Exhibitions/
63
www.carecreations.basf.com in-cosmetics Asia
(p. 60, 62) Dymax Oligomers & Coatings ivan.rahal@reedexpo.co.uk
37
www.dymax-oc.com www.in-cosmeticsasia.com
Bayer Materialscience AG
53
cosmetics@bayermaterialscience.com Excellentia International Rossow USA
17 29
www.bayermaterialscience.com tbuco@excellentiaint.com contact@rossow-usa.com
www.excellentiaint.com www.rossow-usa.com
Berjé, Inc.
57
berje@berjeinc.com Extracts & Ingredients Sabinsa Corp.
52 42
www.berjeinc.com dfondots@morretec.com info@sabinsa.com
www.morretec.com www.sabinsacosmetics.com
Bioland Ltd.
3
bioland@biolandkorea.com Grant Industries SCC California/Suppliers’ Day
1 49
www.biolandkorea.com info@grantinc.com suppliersday@caliscc.org
www.grantinc.com www.caliscc.org
Bloomage Freda Biopharm Co.
11
customer@bloomagefreda.com Ichimaru Pharcos Co. Ltd. SCC New York/
23 9
www.bloomagefreda.com gifu@ichimaru.co.jp Color Cosmetics Symposium
www.ichimaru.co.jp yelena.zolotarsky@bio-amber.com
Brookfield Engineering www.nyscc.org
10
Labs, Inc. Idea Tests
33
info@brookfieldengineering.com v.ribiere@groupeideatests.com Silab
50
www.brookfieldengineering.com www.groupeideatests.com silab@silab.fr
www.silab.fr
Centerchem, Inc. IFSCC (p. 10, 58–59, 60, 62)
C4 61
cosmetics@centerchem.com ifscc.scs@btconnect.com
www.centerchem.com www.ifscc.org Sinerga
13
(p. 60, 62) info@sinerga.it
Ikeda Corp. www.sinerga.it
62
CK Technology info@ikeda-america.com
56
info@ck-techno.com www.ikeda-corp.co.jp Sytheon Ltd.
C3
www.ck-techno.com info@sytheonltd.com
Innospec Ltd. www.sytheonltd.com
41
Clariant International Ltd. americas-pc@innospecinc.com (p. 60, 62)
55
info@clariant.com www.innospecinc.com
www.personalcare.clariant.com (p. 60, 62) TRI-K Industries, Inc.
27
info@tri-k.com
Clinical Research Labs, Inc. Lipotec, LLC www.tri-k.com
43 35
www.crl-inc.com salesoffice@lipotec.com (p. 60, 62)
www.lipotec.com
Corum, Inc. (p. 60) Vevy Europe SpA
45 15
james.lee@corum.com.tw info@vevy.com
www.corum.com.tw www.vevy.com

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What is the article mainly discussing?

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October 2015

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IMPROVEMENT OF VERTICAL WRINKLE AND

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Arlasolve DMI TM Benefits:

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Navigating the Ever-Changing

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Now located at new, expanded

By treating sunscreens Market Intelligence

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Formula 2. Test cream

Table 1. SPF Performance of Each Preparation

W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

Vol. 130, No. 8 | October 2015 Skin Cosmetics & Toiletries® | 19

Formula 3. Test cream plus 3% TiO2

Table 2. SPF Performance with 3% TiO2

W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

Table 3. UVA Protection for Each Formula

W/W% 0% 3% 5% 8% 10% 13% 15% 17% 20%

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Innovative, sustainable, eﬀective ingredients

Table 4. UVA-PF Test Results (ISO-24442, in vivo)

Table 5. SPF Before and After Sun Exposure

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What do We Know About

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BIOACTIVE OLIGOPEPTIDES TO DEFEND SKIN FROM PHOTO-AGING

Maintains healthy, supple skin

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