cosmetics

Project Report
Strategy for the Development of a New Lipstick Formula
Luigi Rigano 1, * and Marta Montoli 2

1 ISPE—Institute of Skin and Product Evaluation, 20125 Milan, Italy

2 Rigano Laboratories S.r.l., 20125 Milan, Italy; montoli@thecosmetologist.com
* Correspondence: rigano@thecosmetologist.com

Abstract: The strategy to adopt for the development of a new lipstick formula requires, as a first
step, the definition of the most important characteristics of a modern product. Successively, the
identification of the key properties of any innovative ingredient is necessary. Then, a comprehension
of the key parameters in the establishment of a stable equilibrium among the different formula
components in the solid state is important. Moreover, it is necessary to study the interactions among
the new ingredients and the other structural components in the formula. Finally, an evaluation of the
sensory properties of the different final formulae for fine-tuning of practical performances needs to be
carefully carried out. In this study, a systematic formulation approach tried to obtain a new lipstick
formula using a new vegetal-derived emollient *(INCLUDING COCO-CAPRYLATE/CAPRATE,
HYDROGENATED OLIVE OIL UNSAPONIFIABLES) with sensorial properties similar to some types
of silicones. Some application trials of the new raw material were carried out. The following aspects
of this ingredient were investigated: (1) Compatibility and thickening with waxes, (2) dispersion
power of pigments, and (3) influence on sensory characteristics of the formulated lipstick. This
new emollient has been shown to improve some aspects of a lipstick formula, in particular shine,
homogeneity, and covering effect. The optimization of the formula, in order to increase the sensation



of softness on the lips, is described. *Plantasens Olive LD SP ECO, supplier Clariant Gmbh.



Citation: Rigano, L.; Montoli, M. Keywords: makeup; lipstick; vegetal raw material; formulation
Strategy for the Development of a
New Lipstick Formula. Cosmetics
2021, 8, 105. https://doi.org/
10.3390/cosmetics8040105 1. Introduction
1.1. Lipstick Formula—Key Requirements
Academic Editor: Enzo Berardesca
As for with makeup products, the main aim of a lipstick formula is to release a colored
Received: 27 September 2021
layer, in this case onto the lips, with a simple and soft application. Even if a fair stick softness
Accepted: 3 November 2021
during distribution is required, an adequate mechanical resistance during application onto
Published: 5 November 2021
the lips should oppose the bending forces involved in this process. The colored trace must
be homogeneous, continuous, without oil stripes (the so-called ‘motorboat effect’), hiding
Publisher’s Note: MDPI stays neutral
the wrinkles of the lips as much as possible. Moreover, the pigmented layer should stay on
with regard to jurisdictional claims in the lips pseudo-mucosa, and keep stable for hours in spite of the continuous movements
published maps and institutional affil- and friction of the lips, not bleeding or diffusing by capillary forces along the wrinkle paths.
iations. The layer must be plastic and elastic in order to follow the skin’s movements, be water and
saliva resistant, not staining easily surfaces that might came into contact with the lips [1].
Safety for the lips and after ingestion must be granted. Shape stability of the stick over time
and at different temperatures, even following transportation in a handbag, is necessary.
Copyright: © 2021 by the authors.
‘Sweating’ droplets of oil on the surface should not appear, even in adverse conditions.
Licensee MDPI, Basel, Switzerland.
Detachment from the holding support of the lipstick case must be absolutely avoided.
This article is an open access article As the stick surface is continuously exposed to atmospheric oxygen, the formula’s ease
distributed under the terms and of rancidity should be minimized. Microbial contamination is highly unlikely in case of
conditions of the Creative Commons anhydrous formulae; nevertheless, the exposed external layer should not support microbial
Attribution (CC BY) license (https:// proliferation following contact with the lips and their resident microflora [2,3].
creativecommons.org/licenses/by/
4.0/).

Cosmetics 2021, 8, 105. https://doi.org/10.3390/cosmetics8040105 https://www.mdpi.com/journal/cosmetics

Cosmetics 2021, 8, 105 2 of 15

1.2. Basic Ingredient Structure of a Lipstick

The indicative composition of a lipstick is described in Table 1.

Table 1. Average composition of a lipstick formula, by ingredients.

Waxes (10–25%)
Butters (10–15%)
Oils (30–50%)
Texturizers and Fillers (8–12%)
Pigments and Pearls (5–20%)
Antioxidants and Preservatives (around 1%)
Parfum (1–2%)
Special Additives (1–5%)

Stable equilibrium among different types of substances is quite a delicate issue. Start-
ing from the key ingredients, the waxes’ lattice provides most of the structural and layering
properties of a lipstick formula. In a strict chemical sense, waxes are esters of long chain
fatty acids with long chain fatty alcohol, but under a cosmetic definition, the term waxes
usually also includes long chain hydrocarbons, as for instance, microcrystalline or polyethy-
lene waxes. The common factor are their ‘waxy’ characteristics, like high melting point,
resistance to friction, layering effect, and chemical and thermal stability. All these are little
polarity ingredients, with limited compatibility with polar oils and insufficient wetting
power for the pigments’ surface, that is usually medium to very polar. Butters or medium
melting point pastes are used to influence the crystalline structure after cooling and pro-
vide a continuum of melting points and viscosity among waxes and fluid oils. Oils, in
lipstick recipes, have a double function. Firstly, they are used to prepare highly viscous
suspensions of thoroughly micronized pigments, keeping solid particles well separated
and avoiding aggregation and sedimentation after wet-milling. Then, oils are used to make
the crystalline lattice of waxes softer and plasticky, providing ease of distribution over
the skin, and controlling shine and softness of the applied layer [4,5]. As a consequence,
the first step when testing a new oil additive is to verify its compatibility with common
lipstick waxes. Successively, the oil’s capability toward pigment dispersion needs to be
analyzed. Then, all the sensorial, stability, and mechanical events after introduction in the
whole formula, as substitute of traditional oil, have to be checked.

2. Materials and Methods

COCO-CAPRYLATE/CAPRATE AND HYDROGENATED OLIVE OIL UNSAPONIFI-
ABLES is a vegetal-derived emollient. Its sensorial properties in the skincare field show
large similarities to the most commonly used silicones.
At room temperature, it is a clear liquid, with a pale yellow color and faint, character-
istic odor. All the other formulation ingredients are commonly used in lipsticks. The list of
these ingredients is described in Table 2.

2.1. Compatibility Trials with Waxes

Compatibility trials have been carried out, both with vegetable and non-vegetable
waxes (Table 3) commonly used in lipsticks, following the same procedure.
The trial procedure implies weighing the selected key wax at two different concentra-
tions: 10% and 25% into the new oil, then heating the blend to the temperature required to
dissolve the wax, under stirring, until a complete solution. The next step is cooling slowly
to room temperature, while stirring. In lipstick formulae, different types of waxes are
frequently used in the blend, in order to obtain a more mechanically resistant solid lattice
at room temperature. Therefore, the behavior of the new oil in blends of three different
waxes was also verified, for a total amount of 15%; each wax was used at 5%. Viscosity
Cosmetics 2021, 8, 105 3 of 15

was measured at 25 ◦ C. Values are taken at three speeds (2.5, 5, and 10 rpm), by using
the Viscosimeter Brookfield RVT (AMETEK GmbH/B.U. Brookfield, Hadamar-Steinbach,
Germany), with Helipath Stand or standard Spindles.

Table 2. Key raw materials, commercial names, suppliers, and INCI.

Trade Name Supplier INCI

Coco-Caprylate/Caprate, Hydrogenated Olive
Plantasens Olive LD SP ECO Clariant
Oil Unsaponifiables
Hombitan FF Venator Uncoated Titanium Dioxide CI 77891
Unipure LC 887 Sensient Brown Iron Oxide CI 77491-77492-77499
Cerabeil Blanche Baerlocher Cera Alba
Candelilla Cera Baerlocher Candelilla Cera
Cerauba T1 Baerlocher Copernicia Cerifera Cera
Plantasens Cosmetic Wax A5 Clariant Hydrogenated Vegetable Oil
Plantasens Crystolive Wax Clariant Olea Europaea Oil Unsaponifiables
Ozokerite T319 Baerlocher Ozokerite
Multiwax ML44H Sonneborn Cera Microcristallina
Belsil SDM 5055 VP Wacker Stearyl Dimethicone
Pelemol ODR Phoenix Chemical Octyldodecyl Ricinoleate
Performalene 500 New Phase Technologies Polyethylene
Limnanthes Alba Seed Oil, Butyrospermum Parkii
Plantasense Carefeel Fresh Clariant
Butter Extract
Supersterol Ester Croda C10-30 Cholesterol/Lanosterol Esters
Ricinus Communis Seed Oil, Hydrogenated Castor Oil,
Plantasens VP R15 Clariant
Copernicia Cerifera Cera
Plantasens Olive Squalane Clariant Squalane
Rootnes Energize Clariant Dicaprylyl Ether, Luffa Cylindrica Root Extract
Velsan SC Clariant Sorbitan Caprylate

Table 3. Waxes commonly used in lipsticks.

Inci Name
Cera Alba
Cera Candelilla
Cera Carnauba
Hydrogenated Vegetable Oil
Olea Europaea Oil Unsaponifiable
Ozokerite
Cera Microcristallina
Stearyl Dimethicone

2.2. Dispersion of Pigments

The study is carried out in order to verify the ability of coco-caprylate/caprate and
hydrogenated olive oil unsaponifiables to wet pigments, in comparison to castor oil, which
is commonly used for the dispersion of pigments and lakes in makeup products.
The chosen mineral pigments and lakes commonly used in makeup products are:
• Uncoated Titanium Dioxide (HOMBITAN FF)
Cosmetics 2021, 8, 105 4 of 15

• Uncoated Zinc Oxide (Z-COTE)

• Brown Iron Oxide (UNIPURE LC 887), a blend of black, red, and yellow iron oxide
• Red Lake (D&C Red N7 Calcium Lake)
Dispersions at 40% solid load were made for the pigments, and at 25% for the lake.
Dispersions were homogenized at room temperature for 10 ◦ C at constant speed
(4000 rpm with Silverson L4R turboemulsifier, Silverson Machines Ltd., Chesham, UK).
Then they were observed under a microscope, after adequate dilution.

2.3. Technical Parameters of Formulas

The following chemico–physical parameters were verified on the obtained blends and
lipstick formulas:
• Viscosity with Brookfield RVT Viscosimeter (AMETEK GmbH/B.U. Brookfield, Hadamar-
Steinbach, Germany), with Helipath stand/standard Spindles;
• Microscopic structure with optical microscope (Optika M-699, OPTIKA S.r.l., Pon-
teranica, Italy) and 300× magnification;
• Drop point measured with the Ubbelhode termometer;
• Determination of breaking load, by applying weights to the lipstick.

3. Results of the Application Trials

3.1. Compatibility with Waxes
These trials allowed to understand the compatibility of coco-caprylate/caprate and
hydrogenated olive oil unsaponifiables with vegetable and non-vegetable waxes and how
they can influence its viscosity at two different concentrations: 10% and 25%. The operation
procedure is described in Paragraph 2.1. The viscosity values of the obtained blends at 10%
of waxes are reported in the following table (Table 4).

Table 4. Viscosity values of the new oil containing 10% waxes at T0.

Viscosity (mPa·s) Spindle 2, Helipath T-C or T-F

Wax
2.5 rpm 5 rpm 10 rpm
Cera Alba 64,000 46,000 25,000
Candelilla Cera 80,000 28,000 16,000
Copernicia Cerifera Cera 800 600 400
Hydrogenated Vegetable Oil 4800 3200 2200
Olea Europaea Oil
640 480 320
Unsaponifiables
Ozokerite 32,000 20,000 14,000
Cera Microcristallina 1360 1080 600
Stearyl Dimethicone 200 160 80

After 24 h, all the gels obtained showed homogeneous appearance. After 2 weeks,
gels with 10% Copernicia Cerifera Cera, hydrogenated vegetable oil, and Olea Europaea
oil unsaponifiables showed evident syneresis. Below, the viscosity values measured of oil
solutions with 25% wax at T0, after 24 h and after 3 months, kept at room temperature, are
shown in Table 5. A gel with 25% Copernicia Cerifera Cera shows an uneven appearance.
It is evident that the new oil offers a good combination of rheological effects at a fairly high
concentration of waxes, even if in some cases, a good thickening effect was also observed
at 10% wax.
Cosmetics 2021, 8, 105 5 of 15

Table 5. Viscosity values of the new oil blended with 25% waxes at T0, T24 h, and after 3 months.

Viscosity (mPa·s) Spindle 2, Helipath T-C or T-F

Wax
2.5 rpm 5 rpm 10 rpm
T0 1,080,000 620,000 310,000
Cera Alba T24 h 1,120,000 540,000 280,000
3 months 1,040,000 600,000 290,000
T0 1,800,000
Candelilla Cera (*) T24 h 2,300,000
3 months 4,900,000
T0 360,000 220,000 150,000
Copernicia Cerifera Cera T24 h 1,000,000 300,000 140,000
3 months 1,800,000 740,000 400,000
T0 220,000 100,000 50,000
Hydrogenated
T24 h 240,000 130,000 100,000
Vegetable Oil
3 months 240,000 100,000 50,000
T0 64,000 34,000 21,000
Olea Europaea Oil
Unsaponifiables T24 h 80,000 40,000 23,000
3 months 76,000 34,000 18,000
T0 680,000 360,000 210,000
Ozokerite T24 h 1,000,000 680,000 390,000
3 months 1,040,000 440,000 220,000
T0 104,000 60,000 34,000
Cera Microcristallina T24 h 112,000 66,000 36,000
3 months 132,000 74,000 43,000
T0 200 160 80
Stearyl Dimethicone T24 h 200 160 80
3 months 200 160 80
(*) Due to the high viscosity of the mix with Candelilla Cera, measurement with Helipath T-F was performed only
at 0.5 rpm.

The viscosity of most blends remained almost stable after three months in samples
kept at room temperature. A significant increase with time was observed for Candelilla
and Copernicia Cerifera waxes. With Stearyl Dimethicone, no increase in viscosity was
observed from 10% to 25%.
No syneresis was observed in any gel at 25% waxes, both after 24 h or 3 months.
Viscosity of the blends remained almost stable after three months at room temperature.
The figures below summarize and highlight the most interesting data:
• Influence of the most compatible waxes at 10% and 25% on the viscosity of the new
oil (Figure 1);
• Viscosity trends over time for gels with 25% waxes (Figure 2).

3.2. Compatibility with Ternary Blends of Waxes

As with makeup formulations, frequently, blends of different waxes are used in order
to obtain increased mechanical properties [6]. Compatibility tests were thus carried out
with blends of three different waxes. Each wax was used at 5%, for a total amount of 15%.
Below are the viscosity values measured for each blend at T0, after 24 h and 3 months at
room temperature (Table 6 and Figure 3).
Cosmetics 2021, 8, x FOR PEER REVIEW 6 of 14
Cosmetics 2021, 8, 105 6 of 15
Cosmetics 2021, 8, x FOR PEER REVIEW 6 of 14

Figure 1. Viscosity values at 2.5 rpm for the most compatible waxes at 10% and 25% at T0 (at 0.5
Figure 1. Viscosity values at 2.5 rpm for the most compatible waxes at 10% and 25% at T0 (at 0.5 rpm
rpm for1.25%
Figure Candellila
Viscosity Cera).
values at 2.5 rpm for the most compatible waxes at 10% and 25% at T0 (at 0.5
for 25% Candellila Cera).
rpm for 25% Candellila Cera).

Figure 2. Trend of viscosity values at 2.5 rpm of 25% wax in oil gels at T0, T24, and after 3 months (at 0.5 rpm for Candelilla
Cera).

3.2. Compatibility with Ternary Blends of Waxes

Figure
Figure 2.
2. Trend ofviscosity
Trend of viscosityvalues
valuesatat2.5
2.5 rpm
rpm ofof 25%
25% waxwax in oil
in oil gelsgels at T0,
at T0, T24,T24,
andand
afterafter 3 months
3 months (at 0.5(at 0.5for
rpm rpm for Candelilla
Candelilla Cera).
Cera). As with makeup formulations, frequently, blends of different waxes are used in order
Table 6. Viscosityto obtain
values of increased
the new oilmechanical
with blends properties [6]. Compatibility
of three waxes testsafter
at T0, T24 h, and were3 thus carried out
months.
with blends of three different waxes. Each
3.2. Compatibility with Ternary Blends of Waxes wax was used at 5%, for a total amount of 15%.
Below are the viscosity values measured for each Viscosity (mPa·s) Helipath T-C or T-B at
blend at T0, after 24 h and 3 months
Wax Blends
room Astemperature
with makeup formulations,
(Table 6 and Figurefrequently,
3). blends of different waxes are used in order
2.5 rpm
to obtain increased mechanical properties [6]. Compatibility 5 rpm tests were thus10carried
rpm out

5% Cera Alba with blends of three different

T0 waxes. Each wax was used at88,000
148,000 5%, for a total amount
47,000of 15%.
5% Candelilla CeraBelow are the viscosity values
T24 h measured for
100,000 each blend at T0, after
58,000 24 h and 3 months at
35,000
5% Copernicia Ceriferaroom
Cera temperature (Table 6 and Figure 3).
3 months 252,000 126,000 71,000
T0 148,000 76,000 38,000
5% Cera Alba
5% Hydrogenated Vegetable Oil T24 h 160,000 82,000 45,000
5% Ozokerite 3 months 112,000 60,000 32,000
Cosmetics 2021, 8, x FOR PEER REVIEW 7 of 14

Cosmetics 2021, 8, 105 Table 6. Viscosity values of the new oil with blends of three waxes at T0, T24 h, and after 3 7 of 15
months.

Viscosity (mPa∙s) Helipath T-C or T-B

Wax Blends
Table 6. Cont. 2.5 rpm 5 rpm 10 rpm
5% Cera Alba T0 148,000 88,000 47,000
5% Candelilla Cera (mPa·s) Helipath
T24 hViscosity100,000 T-C or T-B 35,000
58,000
Wax Blends
5% Copernicia Cerifera Cera 32.5
months
rpm 252,0005 rpm 126,000 71,000
10 rpm
5% Cera Alba T0 148,000 76,000 38,000
T0 56,000 30,000 15,000
5% Hydrogenated Vegetable 5%Oil Hydrogenated Vegetable Oil T24 h 160,000 82,000 45,000
5% Olea Europaea Oil Unsaponifiables 5% OzokeriteT24 h 60,000 34,000 18,000
3 months 112,000 60,000 32,000
5% Ozokerite
5% Hydrogenated3 Vegetable
months Oil 64,000
T0 56,000 32,000 30,000 25,000
15,000
5% Olea Europaea Oil Unsaponifiables
T0 T24
9600h 60,000 5600 34,000 18,000
2800
5% Copernicia Cerifera Cera
5% Ozokerite 3 months 64,000 32,000 25,000
5% Hydrogenated Vegetable Oil T24 h 9600 5600 3600
5% Cera microcristallina 5% Copernicia Cerifera Cera T0 9600 5600 2800
3 months 11,200 6400 4000
5% Hydrogenated Vegetable Oil T24 h 9600 5600 3600
5% Candelilla Cera T0
5% Cera microcristallina 3 40,000
months 11,200 24,000 6400 15,000
4000
5% Olea Europaea Oil Unsaponifiables5% Candelilla Cera
T24 h T0
32,000 40,000 22,000 24,000 15,000
12,000
5% Stearyl Dimethicone5% Olea Europaea Oil Unsaponifiables T24 h 32,000 10,000 22,000 12,000
3 months 18,000 5500
5% Stearyl Dimethicone 3 months 18,000 10,000 5500

Each blend
Each blend proved
provedto
tobe
bestable
stableover
overtime:
time:gels showed
gels showedno no
syneresis or uneven
syneresis appear-
or uneven ap-
ance. The first blend composed of 5% Cera Alba + 5% Candelilla Cera + 5% Copernicia
pearance. The first blend composed of 5% Cera Alba + 5% Candelilla Cera + 5% Copernicia
cerifera Cera
cerifera Cerashowed
showeda aviscosity
viscosity increase
increase after
after 3 months
3 months at room
at room temperature;
temperature; oncon-
on the the
contrary, the one made up of 5% Candelilla Cera + 5% Olea Europaea Oil
trary, the one made up of 5% Candelilla Cera + 5% Olea Europaea Oil Unsaponifialbes + Unsaponifi-
albes
5% + 5% Dimethicone
Stearyl Stearyl Dimethicone
showedshowed a viscosity
a viscosity decrease.decrease.

Figure 3. Trend
Figure 3. of viscosity
Trend of viscosity values
values at
at 2.5
2.5 rpm
rpm of
of blends
blends waxes
waxes in
in oil
oil at
at T0,
T0, T24
T24 h,
h, and
and after
after 33 months.
months.

3.3. Dispersion
Dispersion ofof Pigments
Pigments
The ability
ability of
of the
the new
new oil
oil to
to wet
wet pigments
pigments was
was verified,
verified, having
having castor
castor oil
oil as
as aa bench-
bench-
mark reference
reference oil,
oil,commonly
commonlyused usedfor
forthe
thedispersion
dispersionof of pigments
pigments and and lakes
lakes in lipsticks
in lipsticks for
for its high
its high polarity,
polarity, relative
relative stability,
stability, andand
high high pigment
pigment wetting
wetting power.
power. Moreover,
Moreover, castor
castor oil
oil works
works as aascoupling
a coupling agent
agent between
between non-polar
non-polar waxes
waxes and and polar
polar oils Uncoated
oils [7]. [7]. Uncoated tita-
titanium
nium
dioxide,dioxide,
brownbrown iron oxide,
iron oxide, blend blend of black,
of black, red,yellow
red, and and yellow iron oxides;
iron oxides; Red(D&C
Red Lake Lake
Red N7 Calcium Lake), representing the two categories of pigments used in lipsticks, i.e.,
oxides and lakes, were selected. Dispersions at 40% solid load were prepared for the oxide
pigments, at 25% for the lake. They were homogenized at room temperature for 10 ◦ C at
constant speed (≈4000 rpm) in order to break the pigment agglomerates [8]. Dispersions
Cosmetics 2021, 8, x FOR PEER REVIEW 8 of 14

(D&C Red N7 Calcium Lake), representing the two categories of pigments used in lip-
Cosmetics 2021, 8, 105 8 of 15
sticks, i.e., oxides and lakes, were selected. Dispersions at 40% solid load were prepared
for the oxide pigments, at 25% for the lake. They were homogenized at room temperature
for 10 °C at constant speed (≈4000 rpm) in order to break the pigment agglomerates [8].
Dispersions
were observed were observed
under under a microscope,
a microscope, after adequate after adequate
dilution withdilution with theoil.
the dispersing dispers-
As an
ing oil. As anexample
explanatory explanatory
of theexample
wettingof the wetting
properties properties of coco-caprylate/caprate
of coco-caprylate/caprate and hydrogenated and
hydrogenated olive oil unsaponifiables,
olive oil unsaponifiables, the
the dispersions ofdispersions
40% titanium of 40% titanium
dioxide dioxide
in castor in castor
oil and in the
oil
newand
oilin the
are new oil
shown are shown in(Figure
in comparison comparison
4). (Figure 4).

(a) (b)

(c) (d)
Figure
Figure 4.4.(a)
(a)40% TiO
40% 2 in castor
TiO oil; oil;
2 in castor (b) TiO dispersion
(b) 2TiO in castor
2 dispersion oil after
in castor oil50%
afterdilution (300×); (c)
50% dilution (30040%
×);
TiO 2 in Plantasens
(c) 40% Olive LDOlive
TiO2 in Plantasens SP ECO;
LD SP (d) ECO;
TiO2 dispersion in Plantasens
(d) TiO2 dispersion Olive LD SP
in Plantasens ECO
Olive LDafter 50%
SP ECO
dilution
after 50%(300×).
dilution (300×).

The
The microscope observation
observation revealed
revealedthatthatthe
thedispersion
dispersioninincastor
castoroil
oilisismore
morehomoge-
homo-
geneous, with
neous, with smaller
smaller agglomerates.
agglomerates. Trials
Trials repeated
repeated withwith the selected
the selected ironiron
oxidesoxides
and and the
the lake
lake (not shown)
(not shown) presented
presented similar
similar behaviour.
behaviour. Therefore,
Therefore, it wasitconcluded
was concluded
that thethat
oilthe oil
under
under examination
examination was notwas not than
better bettercastor
than castor
oil for oil
thefor the dispersion
dispersion of pigments.
of pigments.

4. Lipstick
4. Lipstick Formulation
Formulation
The final
The final aim
aim ofof this
this study
study is to create an anhydrous lipstick formula
formula using
using a new
vegetal-derived oil
vegetal-derived oil in
in combination
combination with
with other
other raw
raw materials
materials used
used in
in lipsticks.
lipsticks. For
Forthis
thispur-
pur-
pose, a simple starting model formula was chosen, whose chemico–physical characteristics
pose, a simple starting model formula was chosen, whose chemico–physical characteris-
andand
tics stability are known
stability are known(Table 7). 7).
(Table
Table 7. Initial lipstick formula (Ref.11/21/1).
Table 7. Initial lipstick formula (Ref.11/21/1).
Phase.
Phase. Inci
Inci Name
Name % w/w
% w/w
Ricinus
Ricinus CommunisSeed
Communis SeedOil
Oil 41.55
41.55
CiCi
77891
77891 3.00
3.00
AA
CiCi
15850
15850 2.00
2.00
CiCi
19140
19140 2.00
2.00
Octyldodecyl Ricinoleate 15.00
B Octyldodecyl Ricinoleate 15.00
Bht 0.10
B Bht 0.10
Polyethylene 1.50
Cosmetics 2021, 8, 105 9 of 15

Table 7. Cont.

Phase. Inci Name % w/w

Limnanthes Alba Seed Oil, Butyrospermum Parkii Butter Extract 10.00
Cera Alba 5.00
C Candelilla Cera 6.50
Ozokerite 5.00
C10-30 Cholesterol/Lanosterol Esters 6.50
D Tocopheryl Acetate 1.00
Phenoxyethanol 0.80
E
Vanillin 0.05
100.00

Key features of this formula:

• Pigments dispersed in castor oil;
• Total amount of waxes: 18% including polyethylene wax;
• Orange-red color, with a semi-gloss finish;
• Drop point: 66 ◦ C;
• Breaking load at room temperature: 200 g.

4.1. The Importance of Oils: Formulation Trials

The first change made to the base formula, concerning the fluid ingredients, was the
introduction of the trial oil as replacement of, alternatively (Table 8):
• 10% Castor Oil (Ref.1/21/1A)
• Octyldodecyl Ricinoleate (Ref. 1/21/1B)
• Limnanthes Alba Seed Oil, Butyrospermum Parkii Butter Extract (Ref. 1/21/1C)

Table 8. Lipstick formulae with the new oil substitution.

Phase Inci Name A B C

Ricinus Communis Seed Oil 31.55 41.55 41.55
Ci 77891 3.00 3.00 3.00
A Ci 15850 2.00 2.00 2.00
Ci 19140 2.00 2.00 2.00
Coco-caprylate/Caprate, Hydrogenated Olive
10.00 15.00 10.00
Oil Unsaponifiables
Octyldodecyl Ricinoleate 15.00 - 15.00
B Bht 0.10 0.10 0.10
Polyethylene 1.50 1.50 1.50
Limnanthes Alba Seed Oil, Butyrospermum
10.00 10.00 -
Parkii Butter Extract
Cera Alba 5.00 5.00 5.00
C Candelilla Cera 6.50 6.50 6.50
Ozokerite 5.00 5.00 5.00
C10-30 Cholesterol/Lanosterol Esters 6.50 6.50 6.50
D Tocopheryl Acetate 1.00 1.00 1.00
Phenoxyethanol 0.80 0.80 0.80
E
Vanillin 0.05 0.05 0.05
 Cosmetics 2021, 8, 105 10 of 15

• Drop point: 64 ◦ C, Breaking load: 140 g (Ref. 1/21/1A)

Cosmetics 2021, 8, x FOR PEER REVIEW 10 of 1
• Drop point: 64 ◦ C, Breaking load: 182 g (Ref. 1/21/1B)
• Drop point: 66 ◦ C, Breaking load: 163 g (Ref. 1/21/1C)
The replacement of 10% of castor oil caused a significant reduction in the breaking load.
Moreover,
Moreover, thisthis change
change worsened
worsened the homogeneity
the homogeneity of theontrace
of the trace on the
the skin, skin, compare
compared
to the starting formula. Reference 1/21/1B, where the trial oil replaces Octyldodecyl
to the starting formula. Reference 1/21/1B, where the trial oil replaces Octyldodecyl Rici- Ric
inoleate,
noleate, thethe formula
formula showed
showed better
better spreading
spreading properties.
properties. This change
This change makes applicatio
makes application
easier,
easier, leaving a brighter mark, with very good covering characteristics5).
leaving a brighter mark, with very good covering characteristics (Figure (Figure 5).

Figure5.5.Trace
Figure Trace
of of Starting
Starting Formula
Formula vs. 1/21/1B.
vs. Ref. Ref. 1/21/1B.

4.2.
4.2.Further
FurtherImprovements
Improvements
Successively, additional changes were made to the formula in order to try and obtain
Successively, additional changes were made to the formula in order to try and obtai
further fine improvement of the application results. Changes made are here described by
further fine improvement of the application results. Changes made are here described b
distinguishing some categories of ingredient:
distinguishing some categories of ingredient:
• Oils and soft-solid lipids
•• Waxes
Oils and soft-solid lipids
•• Active
Waxes ingredients
• Active
(a) Oils and softingredients
solid lipids
(a) Oils and softlipids
Oils and soft solidcontribute
lipids to easier spreading, softness, trace brightness and shine. As
a modelOils and soft lipidsthe
for oil replacement, trial replacement
contribute to easierconcerns C10-30softness,
spreading, Cholesterol/Lanosterol
trace brightness an
Esters, an emollient with a soft solid firmness that exhibits excellent spreading ability
shine. As a model for oil replacement, the trial replacement concerns C10-30 Choles
and provides good adhesion properties to anhydrous lipsticks. For testing purposes, we
terol/Lanosterol Esters, an emollient with a soft solid firmness that exhibits excellen
selected the blend Ricinus Communis Seed Oil, Hydrogenated Castor Oil, Copernicia
spreading
Cerifera ability
cera. and provides
This moisturizing good adhesion
mixture properties
shows similar to anhydrous
hydration lipsticks.
and occlusion profile For tes
to petrolatum, having good softening effect and spreading properties [9]. The obtained Casto
ing purposes, we selected the blend Ricinus Communis Seed Oil, Hydrogenated
Oil, Copernicia
lipstick has a dropCerifera 66 ◦ CThis
point of cera. and amoisturizing
breaking loadmixture
of 198 g.shows similar
A greater hydration
covering effect and oc
was observed
clusion with
profile tothis modification.
petrolatum, having good softening effect and spreading properties [9
(b)
TheWaxes
obtained lipstick has a drop point of 66 °C and a breaking load of 198 g. A greate
The total
covering amount
effect wasofobserved
waxes in the formula
with is 18%. Below are their melting points (Table 9).
this modification.
(b) Waxes
Table 9. Melting points of waxes contained in the formula.
The total amount of waxes in the formula is 18%. Below are their melting points (Ta
ble 9). Waxes Melting Points
Cera Alba 63–65 ◦ C
Table 9. Melting points of
Candelilla waxes contained in the formula.
Cera 68–72 ◦ C
Ozokerite 73–76 ◦ C
Waxes Melting Points
Polyethylene Cera Alba 83–91 ◦ C 63–65 °C
Candelilla Cera 68–72 °C
Ozokerite 73–76 °C
Polyethylene 83–91 °C

First change: Replacement of 5% Cera Alba with Hydrogenated Vegetable Oil, wit
Cosmetics 2021, 8, 105 11 of 15

First change: Replacement of 5% Cera Alba with Hydrogenated Vegetable Oil, with a
melting point of 62–72 ◦ C. The resulting lipstick has a melting point of 67 ◦ C and a breaking
load of about 171 g.
Then, we tried to replace 6.5% Candelilla Cera with Olea Europaea Oil Unsaponifi-
ables: the result has a lower melting point (45–56 ◦ C) and the lipsticks obtained had too
soft a structure. The percentage of this last wax was therefore reduced to increase that
of Ozokerite.
In order to reduce the ingredients of synthetic origin, Polyethylene wax replaced by
Copernicia Cerifera Cera, which has an equally high melting point (81–86 ◦ C). However,
it was necessary to increase the percentage of Copernicia Cerifera Cera to 3.5% to obtain
lipsticks with adequate mechanical resistance [10]. Table 10 shows the blend of waxes
selected. The total amount of waxes is now 19%.

Table 10. Selected wax blend.

Inci Name % w/w

Ozokerite 7.00
Hydrogenated Vegetable Oil 5.00
Olea Europaea Oil Unsaponifiables 3.50
Copernicia Cerifera Cera 3.50

The lipsticks so obtained have a melting point of 68 ◦ C and a breaking load of 220 g.
(c) Active ingredients
The so-called ‘active ingredients’ in a lipstick are ingredients which provide additional
benefit to the skin during the long stay of the trace onto the skin. They have been selected
in order to obtain moisturizing and firming properties (Tables 11 and 12) [11,12]:

Table 11. Selected active ingredients.

Inci Name % w/w

Squalane 0.50
Dicaprylyl Ether, Luffa Cylindrica Root Extract 1.00

Below, is the final formula created (Formula 1/21/18) with its manufacturing method.
Manufacturing method:
In appropriate equipment, pre-disperse and mill lakes and pigments in castor oil.
Heat phase A to 85 ◦ C while mixing. In two separate vessels, heat phase B to 95 ◦ C and
phase C to 85 ◦ C while mixing.
Add phase C to phase B while mixing. Then add phase B + C to phase A and keep the
temperature constant to 85 ◦ C. Add ingredients D, E and phase F just before casting into
molds at 80 ◦ C.

Table 12. Final lipstick formula Ref. 1/21/18.

Phase Inci Name % w/w

Ricinus communis seed oil 39.05
Ci 77891 3.00
A
Ci 15850 d&c red n6 barium lake 2.00
Ci 19140 d&c yellow n5 al lake 2.00
Coco-caprylate/caprate, hydrogenated olive oil unsaponifiables 15.00
B
Bht 0.10
Cosmetics 2021, 8, 105 12 of 15

Table 12. Cont.

Phase Inci Name % w/w

Limnanthes alba seed oil, butyrospermum parkii butter extract 10.00
Squalane 0.50
Copernicia cerifera cera 3.50
Hydrogenated vegetable oil 5.00
C
Olea europaea oil unsaponifiable 3.50
Ozokerite 7.00
Cosmetics 2021, 8, x FOR PEER REVIEW Ricinus communis seed oil, hydrogenated castor oil, copernicia 12 of 14
6.50
cerifera wax
D Dicaprylyl ether, luffa cylindrica root extract 1.00
DE Dicaprylyl ether, luffa cylindrica
Tocopheryl acetate root extract 1.00
1.00
E Tocopheryl acetate
Phenoxyethanol 1.00
0.56
Phenoxyethanol
Sorbitan caprylate
0.56
0.24
F
F Sorbitan caprylate 0.24
Vanillin 0.05
Vanillin 0.05

Chemico-physical
Chemico-physicalparameters
parametersofofthe
theformula
formulaafter
after2424hhatatroom
roomtemperature:
temperature:
Drop ◦
Droppoint:
point:68 C; Breaking
68 °C; Breakingload:
load:210
210g.g.The
Theformula
formulaproved
provedstable
stableafter
after22months
monthsinin
glass jars and in plastic case at room temperature, 4 ◦ C, and 42.5 ◦ C.
glass jars and in plastic case at room temperature, 4 °C, and 42.5 °C.
The
Thefinal
finalformula
formulahashasaagreater
greatercovering
coveringeffect
effectthan
thanall
allprevious
previousexperiments,
experiments,with
withaa
more homogeneous mark (Figure
more homogeneous mark (Figure 6). 6).

Figure6.6.Starting
Figure StartingFormula
FormulaofofLipstick
Lipstickvs.
vs.Ref.
Ref.1/21/18
1/21/18 (Final
(Finalformula).
formula).

4.3.
4.3.Sensory
SensoryEvaluation
Evaluationafter
afterApplication
Application
This
Thisparagraph
paragraphreports
reports thethe
sensory evaluations
sensory evaluationscarried out for
carried outthe
forformulated lipsticks
the formulated lip-
by an expert
sticks by an panel,
expertconsisting of four subjects.
panel, consisting Due to the
of four subjects. Duesmall number
to the of evaluators,
small number the
of evalua-
evaluation scale was scale
tors, the evaluation highly reduced.
was highly In particular,
reduced. we compared:
In particular, we compared:
•• Starting
Startingformula
formula(Formula
(Formula1)1)vs. vs.Ref.
Ref.1/21/1B (Formula 2,
1/21/1B (Formula 2, with
with 15%
15% of
of the
the new
new oil)
oil)
•• Starting formula (Formula 1) vs. Ref. 1/21/18 (Formula 3, with all fine adjustments).
Starting formula (Formula 1) vs. Ref. 1/21/18 (Formula 3, with all fine adjustments).
Tables
Tables1313and
and1414show
showthe theanalyzed
analyzedparameters
parametersfor foreach
eachformula.
formula.
The introduction of the new oil gives the lipstick a greater covering effect, with a
smoother sensation ofonthethe
Table 13. Evaluation lipsformula
initial and a vs.
more
Ref.homogeneous
1/21/1B. mark. A numerical value is
assigned to the judgments expressed for each parameter, obtaining the following scale:
Parameter
1 = Inadequate; 2 = Poor; 3 = Fair; 4 =Starting
Good; 5 Formula
= Excellent REF. 1/21/1B
Ease
The of application
results are shown in Figure 7. Good Good
Homogeneity of the mark Good Good/Excellent
Covering effect Poor Good
Shine Fair/Good Good
Sensation on the lips Fair/Good Good
Cosmetics 2021, 8, 105 13 of 15

Table 13. Evaluation of the initial formula vs. Ref. 1/21/1B.

Parameter Starting Formula REF. 1/21/1B

Ease of application Good Good
Homogeneity of the mark Good Good/Excellent
Covering effect Poor Good
Shine Fair/Good Good
Sensation on the lips Fair/Good Good
No-transfer effect Fair Good
Cosmetics 2021, 8, x FOR PEER REVIEW 13 of 14
Long-lasting effect Good Good

Figure7.7.Initial
Figure Initialformula
formulavs.
vs.Ref.
Ref. 1/21/1B
1/21/1B (with
(with15%
15%new
newoil).
oil).

Table14.
Table 14.Evaluation
Evaluationofofthe
theinitial
initialformula
formulavs.
vs.Ref.
Ref.1/21/18
1/21/18 (final
(final formula).
formula).
Parameter
Parameter StartingFormula
Starting Formula REF.1/21/18
REF. 1/21/18
Ease of application Good Good
Ease of application Good Good
Homogeneity of the mark Good Excellent
Homogeneity of the mark Good Excellent
Covering effect Poor Excellent
Covering effect Poor Excellent
Shine Fair/Good Good
Shine
Sensation on the lips Fair/Good
Fair/Good Good
Good/Excellent
Sensation
No-transferthe
on lips
effect Fair/Good
Fair Good/Excellent
Good
Long-lasting effect
No-transfer effect Good
Fair Good
Good
Long-lasting effect Good Good
The final formula Ref. 1/21/18 shows a higher covering effect, with a more homoge-
neous and shiny mark, giving a smoother and softer sensation on the lips. The sensorial
The final formula Ref. 1/21/18 shows a higher covering effect, with a more homoge-
results are shown in Figure 8.
neous and shiny mark, giving a smoother and softer sensation on the lips. The sensorial
results are shown in Figure 8.
 Sensation on the lips Fair/Good Good/Excellent
No-transfer effect Fair Good
Long-lasting effect Good Good

Cosmetics 2021, 8, 105 The final formula Ref. 1/21/18 shows a higher covering effect, with a more homoge-
14 of 15
neous and shiny mark, giving a smoother and softer sensation on the lips. The sensorial
results are shown in Figure 8.

Figure 8.
Figure 8. Initial
Initial formula
formula vs.
vs. Ref.
Ref. 1/21/18
1/21/18 (final
(finalformula).
formula).

5. Conclusions
The study conducted in order to understand the formulation strategy necessary to use
a new vegetal oil that could help develop a new lipstick formula allows to underline the
following aspects:
• The new ingredient showed good compatibility with the tested waxes;
• gels obtained with 10% of Cera Alba, Candelilla Cera, Ozokerite, Cera Microcristallina
and Stearyl Dimethicone in the test oil did not show syneresis over time;
• at 25% wax in the oil, no gels showed syneresis;
• good thickening effect observed with Candelilla Cera and Copernicia Cerifera Cera;
• the new oil does not have pigment-wetting properties comparable to castor oil; how-
ever, with titanium dioxide and the tested lake, it was possible to obtain homogeneous
and quite fluid dispersions;
• the introduction of the new oil in a lipstick leads to improvements in terms of homo-
geneity of the mark, shine, and covering effect;
• it was possible to obtain a softer and smoother sensation on the lips by making some
small additional changes to the developed formula.

Author Contributions: Conceptualization, L.R. and M.M.; methodology, L.R. and M.M.; validation,
L.R.; formal analysis, M.M.; investigation, L.R. and M.M.; resources, L.R. and M.M.; data curation,
L.R. and M.M.; writing—original draft preparation, L.R. and M.M.; writing—review and editing, L.R.
and M.M.; supervision, L.R.; project administration, L.R. All authors have read and agreed to the
published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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