Abstract: This invention relates to a composition having a yogurt-like texture comprising : - a fatty phase dispersed in a continuous aqueous phase , said continuous aqueous phase comprising at least three polyols, and - at least three crosslinked or non-crosslinked copolymers comprising 2-acrylamido 2-methyl propane sulfonic acid units. The invention also relates to a process for preparing such a composition, performed at room temperature.
The present invention relates to cosmetic compositions that are useful for personal
5 skin care.
The development of formulations dedicated to caring for and/or making up the skin
and/or lips, is permanent. Said formulations have to show satisfactory properties in terms
of application, such as easy usage, and also in terms of sensory, such as hydration and/or
10 moisturizing feeling after application.
The skin is the protective barrier for the human body. It protects the interior of the
body from physical injury (such as trauma) and biological injury (such as bacteria, viruses
or fungi). The skin of the human body comprises the dermis and the epidermis. The
15 epidermis is the top most layer of the skin, and its superficial layer is called the stratum
corneum.
20
25
Moisturization is provided to the skin by the water in the deep-lying layers and by
perspiration. Cutaneous moisturization disorders, and especially skin dryness, are often
observed with age and/or changes in climate. However, such conditions may also be
manifested in young individuals.
A wide variety of cosmetic compositions have been used to care for the skin, in
particular to provide moisturizing or hydration to the skin. Some of these compositions
present a yogurt-like texture: they look heavy, shiny and greasy, but they are .light once
applied onto skin. Such compositions are typically oil-in-water emulsions, which use
emulsifiers such as fatty acids, fatty esters or fatty alcohols for emulsification. However,
said emulsifiers represent a certain amount of the total solid content of the composition
(typically from 5 to 10%), and necessary involve a heating step in the manufacturing
process of the compositions (also called "hot process").
There is thus a need to formulate a composition for caring for the skin, particularly a
30 composition showing a yogurt-like texture, which has good cosmetic properties, in
particular moisturizing and/or hydration and/or softening of the skin without greasy
feelings. There is a need to formulate a composition as described above, which is stable,
not sticky and not oily, and easy to spread.
Besides, there is a need for such a composition which can be processed at room
35 temperature.
2
It is therefore desirable to provide stable skin care compositions that present
excellent application and sensory characteristics.
The Applicant has now discovered that it is possible to formulate such compositions
5 having the desired properties as described above.
Specifically, the Applicant has discovered that it is possible to formulate
compositions for caring for and/or making up of keratin materials, which are stable, nonsticky,
non-oily, which may be processed at room temperature (i.e. around 25 to 30.C),
and which confer moisturization, hydration and/or softening after application onto skin.
10 Said compositions comprise a unique combination of"three specific polymers. Moreover,
said compositions present a yogurt-like texture.
Accordingly, the present invention relates to a composition, preferably a cosmetic
composition, comprising:
15 - a fatty phase dispersed in a continuous aqueous phase, said continuous aqueous
20
phase comprising at least three polyols, and
- at least three crosslinked or non-crosslinked copolymers comprising 2-acrylamido
2-methyl propane sulfonic acid units (AMPS®).
The composition of the invention is thus in form of an oil-in-water (0/W) emulsion.
The composition of the invention is very easy to spread, while bringing a softening
and moisturizing feeling after application. It presents a yogurt-like texture. Said
composition is stable, and is processed at room temperature, thus does not use a hot
25 process. Finally, said composition is substantially free of emulsifiers.
By "substantially free of emulsifiers", it is meant that the composition of the invention
comprises less than 2% by weight, preferably less than 1% by weight, more preferably
less than 0.5% by weight of the total composition, of emulsifiers. More preferably, the
composition of the invention is devoid of emulsifiers.
30 By "stable", it is meant that the composition of the invention does not show any
35
sedimentation (i.e. collection of the fatty globules at the bottom of the container) or
dephasing (i.e. separation of the aqueous and fatty phases) over time, especially during
one month, preferably during two months, under different temperatures (4·c, 3rc and
45°C).
3
Other subjects and characteristics, aspects and advantages of the invention will
emerge even more clearly on reading the description and the examples that follows.
In that which follows and unless otherwise indicated, the limits of a range of
values are included within this range, in particular in the expressions "of between" and
5 "ranging from ... to ... ".
Moreover, the expression "at least one" used in the present description is
equivalent to the expression "one or more".
Throughout the instant application, the term "comprising" is to be interpreted as
encompassing all specifically mentioned features as well optional, additional, unspecified
10 ones. As used herein, the use of the term "comprising" also discloses the embodiment
wherein no features other than the specifically mentioned features are present (i.e.
"consisting of').
15
20
Aqueous phase
The composition of the invention comprises a continuous aqueous phase, which
comprises at least three polyols.
Said aqueous phase is preferably present in an amount ranging from 1 0% to 99%
by weight, more preferably from 20% to 95% by weight, and even more preferably from
50% to 90% by weight of the total weight of the composition.
The composition of the invention preferably comprises water. Water is preferably
present in the composition of the present invention in an amount ranging from 1% to 85%
by weight, preferably from 5% to 82% by weight, more preferably from 10% to 80% by
weight, relative to the total weight of the composition.
The polyols may be chosen from polyols having from 2 to 20 carbon atoms,
25 preferably from 2 to 10 carbon atoms, and preferentially having from 2 to 6 carbon atoms,
such as glycerol, propylene glycol, butylene glycol, pentylene glycol, hexylene glycol,
caprylylglycol, dipropylene glycol and diethylene glycol. Preferably, the continuous
aqueous phase comprises three polyols, which are glycerol, butylene glycol and pentylene
glycol.
30 The polyols may be present in the composition of the present invention in an amount
ranging from 1% to 30% by weight, preferably from 3% to 20% by weight, more preferably
from 4% to 10% by weight, relative to the total weight of the composition.
Preferably, when the polyols are glycerol, butylene glycol and pentylene glycol, the
amounts of butylene glycol and pentylene glycol are identical. Preferably, when the
35 polyols are glycerol, butylene glycol and pentylene glycol, the weight ratios of glycerol :
butylene glycol: pentylene glycol are comprised between 2-4: 0.8-1.2: 0.8-1.2.
4
The continuous aqueous phase may further comprise at least one organic solvent
miscible with water different from polyols. Said organic solvent miscible with water (at
room temperature 25°C) may be chosen from monoalcohols having from 2 to 6 carbon
atoms such as ethanol, isopropanol; glycol ethers (notably having from 3 to 16 carbon
5 atoms) such as mono-, di- or tri- propylene glycol (C,-C.}alkyl ethers, mono-, di- or
tri-ethylene glycol (C1-C4) alkyl ethers and mixtures thereof.
10
Preferably, the continuous aqueous phase of the composition of the invention
comprises water and a mixture of glycerol, butylene glycol and pentylene glycoL
AMPS® copolymers
The composition of the invention comprises at least three crosslinked or noncrosslinked
copolymers comprising 2-acrylamido 2-methyl propane sulfonic acid units
(AMPS®). Said three copolymers are different one from the others.
15 In the present application, the expression "copolymer comprising 2-acrylamido-2-
20
methylpropanesulphonic acid units" (AMPS®) is intended to mean copolymer of AMPS®
with a monomer different from AMPS®. Said AMPS® copolymers may be both crosslinked
or non-crosslinked copolymers.
They are water-soluble, water-dispersible or water-swellable copolymers.
Preferably, the AMPS® copolymers used in accordance with the invention may be
partially or completely neutralized with an inorganic base (such as sodium hydroxide,
potassium hydroxide or aqueous ammonia) or an organic base such as mono-, di- or
triethanolamine, an aminomethylpropanediol, N-methylglucamine or basic amino acids
such as arginine and lysine, and mixtures of these compounds. They are generally
25 neutralized. In the present invention, the term "neutralized" is intended to mean polymers
that have been completely or almost completely neutralized, i.e. at least 90% neutralized.
The AMPS® copolymers used in the composition of the invention generally have a
number-average molecular weight ranging from 1000 to 20 000 000 g/mol, preferably
30 ranging from 20 000 to 5 000 000, and even more preferably from 100 000 to 1 500 000
g/moL
When the copolymers are crosslinked, the crosslinking agents may be chosen from
compounds with an olefinic polyunsaturation commonly used for crosslinking polymers
35 obtained by radical polymerization. As crosslinking agents, mention may, for example, be
made of divinylbenzene, diallyl ether, dipropylene glycol diallyl ether, polyglycol diallyl
5
ethers, triethylene glycol divinyl ether, hydroquinone diallyl ether, ethylene glycol
di(meth)acrylate, tetraethylene glycol di(meth)acrylate, trimethylolpropane triacrylate,
methylenebisacrylamide, methylenebismethacrylamide, triallylamine, triallyl cyanurate,
diallyl maleate, tetraallylethylenediamine, tetraallyloxyethane, trimethylolpropane diallyl
5 ether, allyl (meth)acrylate, allyl ethers of alcohols ofthe sugar series, or other allyl or vinyl
ethers of polyfunctional alcohols, and also allyl esters of phosphoric acid derivatives
and/or vinylphosphonic acid derivatives, or mixtures of these compounds.
10
15
20
The degree of crosslinking generally ranges from 0.01 to 10 mol %, and more
particularly from 0.2 to 2 mol %, relative to the polymer.
The 2-acrylamido-2-methylpropanesulphonic acid (AMPS®) copolymers of the
invention preferably comprise units of general formula (1):
(I)
in which X+ denotes a proton, an alkali metal cation, an alkaline earth metal cation
or the ammonium ion, it being possible for no more than 10 mol% of the X+ cations to be
H+ protons;
and crosslinking units originating from at least one monomer having at least two
olefinic double bonds.
The AMPS® copolymers that can be used in the composition of the invention may
be chosen in particular from:
- crosslinked copolymers of acrylamide or methacrylamide and of 2-acrylamido-2-
methyl propane sulfonate such as that used in the commercial product Sepigel 305 (CTFA
name: polyacrylamide I C13-C14 isoparaffin I Laureth-7) or one used in the commercial
25 product sold under the name SIMULGEL 600 (CTFA name: Acrylamide I Sodium
Acryloyldimethyltaurate I isohexadecane I polysorbate-SO) by Seppic;
- copolymers of AMPS® and vinylpyrrolidone or vinylformamide, preferably
crosslinked, such as that used in the commercial product sold under the name Aristoflex
AVC by Clariant (CTFA name: Ammonium acryloyldimethyltaurateNP Copolymer) but
30 neutralized by sodium hydroxide or potassium hydroxide, or one used in the commercial
d
li
I
6
product sold under the name Aristoflex AVS by Clariant (CTFA name: Sodium
AcryloyldimethyltaurateNP Crosspolymer); and
- copolymers of AMPS® and sodium acrylate, such as the copolymer AMPS® I
sodium acrylate as used in the commercial product sold under the name SIMULGEL EG
5 by the company SEPPIC, which is a copolymer of acrylic acidlacrylamido-2-
methylpropanesulphonic acid in the form of a sodium salt in an inverse emulsion at 45% in
isohexadecanelwater (CTFA name: Sodium Acrylate I Sodium acryloyldimethyltaurate I
lsohexadecane I Polysorbate-SO). ·
10 Preferably, the composition of the. invention comprises at least one copolymer of
15
20
25
30
AMPS® and vinylpyrrolidone or vinylformamide, preferably vinylpyrrolidone.
Preferably, the 2-acrylamido-2-methylpropanesulphonic acid copolymers are a
mixture of:
- at least one crosslinked copolymer of acrylamide or methacrylamide and of
AMPS®;
- at least one copolymer of AMPS® and vinylpyrrolidone or vinylformamide,
preferably vinylpyrrolidone; and
- at least one copolymer of AMPS® and sodium acrylate.
AMPS® copolymers according to the invention are generally present in amounts of
active material ranging from 0.01 to 20% by weight, more preferably from 0.1 to 10% by
weight, even more preferably from 0.5 to 5% by weight and more particularly from 0.8 to
2% by weight relative to the total weight of the composition.
Preferably, AMPS® copolymers according to the invention are present in a weight
ratio of active material of (crosslinked copolymerof acrylamide or methacrylamide and of
AMPS®) : (copolymer of AMPS® and vinylpyrrolidone or vinylformamide) : (copolymer of
AMPS® and sodium acrylate) ranging from 2-3: 8-10: 2-3.
Fatty phase
The composition of the invention further comprises a dispersed fatty phase.
The fatty phase is present in an amount ranging from 1% to 60% by weight,
preferably from 3% to 40% by weight, more preferably from 5% to 30% by weight, more
preferably from 5% to 20% by weight, relative to the total weight of the composition.
35 Said fatty phase preferably comprises at least one oil. The oil can be volatile or nonvolatile.
7
The term "oil" means a water-immiscible non-aqueous compound that is liquid at
room temperature (25°C) and at atmospheric pressure (760 mmHg).
The term "non-volatile oil" means an oil that remains on keratin materials at room
temperature and atmospheric pressure for at least several hours and that especially has a
5 vapour pressure of less than 1 o·3 mmHg (0.13 Pa). A non-volatile oil may also be defined
as having an evaporation rate such that, under the conditions defined previously, the
amount evaporated after 30 minutes is less than 0.07 mg/cm2
.
10
These oils may be of plant, mineral or synthetic origin.
Preferably, said oil is chosen from hydrocarbonated, silicone or fluorinated oils.
The term "hydrocarbon-based oil" or "hydrocarbonated oil" means an oil formed
essentially from, or even constituted by, carbon and hydrogen atoms, and optionally 0
and N atomes, and free of Si and F heteroatoms. Such oil can contain alcohol, ester,
ether, carboxylic acid, amine and/or amide groups.
The term "silicone oil" means an oil containing at least one silicon atom, especially
15 containing Si-0 groups.
20
The term "fluorinated oil" means an oil containing at least one fluorine atom,
Preferably, the oil is selected from hydrocarbonated oils, preferably non-volatile.
The oil can be, for example, present in an amount ranging from 0.01% to 50% by
weight, preferably from 0.1% to 30% by weight, more preferably from 0.5% to 10% by
weight, relative to the total weight of the composition.
Mention may be made, for example, of hydrocarbon-based volatile oils having from
8 to 16 carbon atoms and mixtures thereof and especially branched C8-C16 alkanes such
as C8-C16 isoalkanes (also known as isoparaffins), isododecane, isodecane,
isohexadecane and, for example, the oils sold under the trade names lsopar or Permethyl,
25 C8-C16 branched esters such as isohexyl neopentanoate and mixtures thereof.
lsododecane or isohexadecane are preferred.
As non-volatile oils, mention may be made of:
- hydrocarbon-based oils of mineral or synthetic origin, such as linear or branched
30 hydrocarbons, for instance liquid paraffin or its derivatives, liquid petroleum jelly,
'
polydecenes, hydrogenated polyisobutene such as Parleam sold by the company Nippon
Oil Fats, squalane of synthetic or plant origin;
- hydrocarbon-based oils of plant origin based on triglycerides made up of esters of
fatty acids and of glycerol, the fatty acids of which may have varied chain lengths, it being
35 possible for the latter to be linear or branched, and saturated or unsaturated, in particular
the triglycerides of a fatty acid containing in particular from 4 to 22 carbon atoms, for
8
instance heptanoic acid triglycerides, octanoic acid triglycerides and capric/caprylic acid
triglycerides, or else hydroxylated triglycerides, such as sweet almond oil, calophyllum oil,
palm oil, grape seed oil, sesame oil, arara oil, rapeseed oil, sunflower oil, cottonseed oil,
apricot oil, castor oil, alfalfa oil, marrow oil, blackcurrant oil, macadamia oil, muscat rose
5 oil, hazelnut oil, coriander oil, avocado oil, jojoba oil, olive oil, cereal (maize, wheat,
barley, rye) germ oil, shea butter oil; esters of fatty acids, in particular having from 4 to 22
carbon atoms, and in particular of octanoic acid, of heptanoic acid, of lanolic acid, of oleic
acid, of lauric acid or of stearic acid, such as propylene glycol dioctanoate, propylene
glycol monoisostearate, polyglyceryl-2 diisostearate, neopentyl glycol diheptanoate;
10 - synthetic esters of formula R1COOR2 in which R1 represents the residue of a
linear or branched higher fatty acid containing from 7 to 40 carbon atoms and R2
represents a branched hydrocarbon-based chain containing from 3 to 40 carbon atoms,
for instance purcellin oil (cetostearyl octanoate), isononyl isononanoate, C12 to C15
alcohol benzoate, 2-ethylhexyl palmitate, 2-octyldodecyl stearate, 2-octyldodecyl erucate,
15 isostearyl isostearate, 2-octyldodecyl benzoate, octanoates, decanoates or ricinoleates of
alcohols or of polyalcohols, isopropyl myristate, isopropyl palmitate, butyl stearate, hexyl
laurate, diisopropyl adipate, 2-ethylhexyl palmitate, 2-hexyldecyl laurate, 2-octyldecyl
palmitate, 2-octyldodecyl myristate, 2-diethylhexyl succinate, diisostearyl malate, isodecyl
neopentanoate, hydroxylated esters such as isostearyl lactate, octyl hydroxystearate,
20 octyldodecyl hydroxystearate, diisostearyl malate, triisocetyl citrate, glyceryl or diglyceryl
triisostearate; diethylene glycol diisononanoate; pentaerythritol esters; esters of aromatic
acids and of alcohols containing from 4 to 22 carbon atoms, in particular tridecyl
trimellitate;
- C8-C26 higher fatty acids such as myristic acid, oleic acid, linoleic acid, linolenic
25 acid or isostearic acid;
- C8-C26 higher fatty alcohols such as oleyl alcohol, linoleyl alcohol, linolenyl
alcohol, isostearyl alcohol or octyldodecanol;
- synthetic ethers containing at least 7 carbon atoms;
- silicone oils such as linear polydimethylsiloxanes (PDMSs) that are liquid at
30 ambient temperature, and that are optionally phenylated, such as phenyltrimethicones,
phenyltrimethylsiloxydiphenylsiloxanes, diphenyl dimethicones, diphenylmethyldiphenyltrisiloxanes,
liquid 2-phenylethyltrimethyl-siloxysilicates, optionally substituted
with aliphatic and/or aromatic groups, for instance alkyl, alkoxy or phenyl groups, which
are pendent and/or at the end of a silicone chain, these groups containing from 2 to 24
35 carbon atoms, and optionally fluorinated, or with functional groups such as hydroxyl, thiol
and/or amine groups; polysiloxanes modified with fatty acids or fatty alcohols or
5
9
polyoxyalkylenes, such as dimethicone copolyols or alkyl methicone copolyols; liquid
fluorosilicones;
- and mixtures thereof.
According to a particularly preferred embodiment, the present invention relates to
a composition in form of an oil-in-water emulsion, comprising:
- from 70% to 90% by weight of the weight of the composition of a mixture of water,
glycerol, butylene glycol and pentylene glycol;
-from 5% to 15% by weight of at least one oil;
10 - from 0.1% to 1% by weight of at .least one crosslinked copolymer of acrylamide or
methacrylamide and of AMPS®;
- from 0.1% to 1.5% by weight of at least one copolymer of AMPS® and
vinylpyrrolidone or vinylformamide; and
- from 0.1% to 1% by weight of at least one copolymer of AMPS® and sodium
15 acrylate.
Additional ingredients
The composition of the invention may comprise at least one additive, such as
fragrances, preservatives, active agents, vitamins, pH regulators and/or fillers.
20 A person skilled in the art can adjust the type and amount of additives present in the
25
compositions according to the invention by means of routine operations, so that the
desired cosmetic properties and stability properties for these compositions are not
affected by the additives.
The filler may be organic or mineral. Among the mineral fillers that can be used in
the compositions according to the invention, mention may be made of talc, mica, silica,
kaolin or bentone. Among the organic fillers, mention may be made of polyamide powders
(Nylon® Orgasol from Atochem), polyalanine and polyethylene powders,
polytetrafluoroethylene (Teflon®) powders, lauroyllysine, tetrafluoroethylene polymer
powders, hollow polymer microspheres, such as Expancel (Nobel lndustrie), metal soaps
30 derived from organic carboxylic acids containing from 8 to 22 carbon atoms, preferably
from 12 to 18 carbon atoms, for example zinc stearate, magnesium stearate or lithium
stearate, zinc Ia urate or magnesium myristate.
Methods and use
10
According to an embodiment, the present invention relates to a non-therapeutic
method for treating a keratin material, comprising the step of applying the composition of
the present invention to the keratin material.
Preferably the present invention relates to a method for caring for the skin,
5 comprising the step of applying the composition of the present invention to the skin.
10
15
20
25
According to another embodiment, the invention relates to the use of a composition
of the present invention for moisturizing a keratin material, especially the skin.
The present invention also relates to a process for preparing a composition of the
invention, comprising the steps of:
a) mixing at least three glycols and at least one crosslinked or non-crosslinked
copolymer comprising 2-acrylamido 2-methyl propane sulfonic acid units, in order
to obtain an aqueous phase, at room temperature;
b) mixing fatty components and at least one crosslinked or non-crosslinked
copolymer comprising 2-acrylamido 2-methyl propane sulfonic acid units, in order
to obtain a fatty phase, at room temperature; and
c) introducing the fatty phase obtained in step b) into the aqueous phase obtained in
step a), in order to obtain an oil-in-water emulsion.
Such a process is notably exemplified in example 1 below.
The following examples serve to illustrate the invention without, however, being
limiting in nature.
EXAMPLES
Example 1: Preparation of compositions according to the present invention
Formulas A and B according to the invention were prepared according to the
amounts given in the table below. The amounts are given in % by weight of the total
30 composition.
Formula Formula
Commercial A B
Phase Name (INCI) Amount Amount
name
(%w/w) (% w/w)
A1 WATER Aqua Qsp 100 Qsp 100
BHT NIPANOX BHT 0.20 0.20
ll i!
II
I. I'
I
:l
!l
ji
I
I
i11
PENTYLENE GLYCOL
616751
HYDROLITE-5 1.00 2.00
BUTYLENE GLYCOL
1 ,3 Butylene
Glycol 1.00 2.00
NIACINAMIDE
USP FINE
GRANULAR 3.00 3.00
CAPRYLOYL SALICYLIC ACID MEXORYL SAB 0.10 0.10
GLYCERIN Glycerin CP {MB) 3.00 5.00
SODIUM BENZOATE
Sodium benzoate
COLUMNAR 0.20 0.20
DISODIUM EDTA EDTA-2NA 0.20 0.20
A2 TITANIUM DIOXIDE Selected A- HRC 0.80 0.80
81 DIMETHICONE Belsyldm 5+ 4.00 4.00
ISOHEXADECANE Arlamol HD 2.00 2.00
CAPRYLIC/CAPRIC TRIGLYCERIDE
WLFARESTER
2.00 2.00
• .. • MCT7030
TITANIUM DIOXIDE (and) DISODIUM
STEAROYL GLUTAMATE (and) NAI-TA0-77891 0.20 0.20
ALUMINUM HYDROXIDE
CAPRYL YL GLYCOL Dermosoft Octiol 0.20 0.20
DL-ALPHA
TOCOPHERYLACETATE
TOCOPHERYL
ACETATE 0.10 0.10
(0420085)
SODIUM
82 ACRYLOYLDIMETHYL TAURATENP Aristoflex AVS® 1.00 1.00
CROSSPOLYMER
SODIUM ACRYLATE/SODIUM
c ACRYLOYLDIMETHYL TAURATE Simulgel EG® 0.70 0.70
COPOLYMER {and) ISOHEXADECANE
{and) POLYSORBATE 80
D
POLYACRYLAMIDE {and) C13-14
Sepigel 305® 0.70 0.70
ISOPARAFFIN (and) LAURETH-7
E PHENOXYETHANOL Sepicide LD 0.70 0.70
F
CITRUS LIMON (LEMON) FRUIT
Secrets DE Citron 0.01 0.01 EXTRACT
BIFIDA FERMENT LYSATE
Repair complex
CLRPF 0.01 0.01
Phytokine
HYDROLYZED SOY PROTEIN Hydrolyte 5 0.01 0.01
REFA0092
ASCORBYL GLUCOSIDE AA2G 0.20 0.20
TRIETHANOLAMINE
Triethanolamine
99.0% CR C 7 0.25 0.25
WATER Aqua 10.00 10.00
G SILICA Sunsphere H 51 0.20 0.20
H TALC
Luzenac pharma
1.00 1.00
M
I FRAGRANCE
Night Rescue
Mod 1 0.30 0.30
The process for preparing formulas A and B is as follows:
1. The ingredients of phase A 1 are mixed in manufacturing vessel. The mixture is
homogenized for 5-7 mins under homogenizer at speed of 800-1200 RPM, at room
5 temperature around 25-30'C);
5
12
2. The ingredient of A2. is added to phase A 1 , the mixture is stirred and homogenized for
8-10 mins.
3. The ingredients of phase 81 are put in another vessel, mixed and homogenized at
1200-1500 RPM, for 5 mins. Then phase 82 is added to phase 81, and the mixture is
homogenized for 10 min at 1500-2000 RPM. This results in phase mixture B;
4. Phases C & Dare added, one after the other, to the mixture of phase A1+A2. The
mixture is stirred and homogenized for 5 min after each addition. The mixture will start
thickening, turn like thin lotion. This results in phase mixture A;
5. Then phase mixture B is added to phase mixture A. This will start the emulsification,
10 resulting in thickening of the mixture. The emulsion is stirred and homogenized for 20 min
at 2000-2100 RPM, at room temperature;
15
20
6. After emulsification, the mixture will turn into thick glossy cream. After that phase E is
added slowly to emulsion, and stirred;
7. Prepare Phase F by adding all the actives & extract in water. Then the blend is
neutralized with triethanolamine;
8. Phase F is added to above emulsion (obtained in 6) at 1200-1500 RPM, then stirred
and mixed;
9. Silica (phase G) is added to above, stirred and mixed;
10. Talc (phase H) is added to above, stirred and mixed;
11. Finally fragrance (phase I) is added to above, stirred and mixed.
Formula B is tested in a corridor test:
Based on a corridor check amongst 5 models, formula B received positive feedbacks and
no gross negative mentioned (no irritation or strong dislike).
25 The method was as follows:
• 5 women aged 20-30 years old, users of night cream
• Monadic, 2 days of placement with 1x of minimum usage I day
• Skin type: Mix- Oily/Dry-normal, no very sensitive skin
3Q The main reasons of liking are:
• The soft cream texture, which eases the spreading process
• Pleasant nature of fragrance - fruity type of scent
• The light, fresh feeling on skin.
35
I
I
I
i!l
I
Before is
Application bouncy
Pleasant nature of
fragrance, with JR
intensity
13
Consistency is too watery
During
Application
Easy to spread Wet sensation lingered for 5-10 mins post application
After
Application
(Skin feel &
look)
Light-watery
sensation
Light feeling on skin
Slight fresh, cooling
sensation
Thin oil layer stayed on hands
Not moist enough for a night cream
Example 2: Comparative formulas and stabilitv study
Comparative formulas C to E were prepared according to the amounts given in the
5 table below. The amounts are given in % by weight of the total composition.
Comparative Comparative Comparati
Formulae Formula D ve
Phase Name (INC I)
Commercial Amount(% Amount(% FormulaE
name w/w) w/w) Amount(%
w/w)
A1 WATER Aqua Qsp 100 Qsp 100 Qsp 100
BHT
NIPANOX 0.20 0.20 0.20
BHT
PENTYLENE GLYCOL
616751 2.00 2.00 2.00 HYDROLITE-5
BUTYLENE GLYCOL 1 ,3 Butylene 2.00 2.00 2.00
Glycol
NIACINAMIDE
USP FINE 3.00 3.00 3.00
GRANULAR
CAPRYLOYL MEXORYL
0.10 0.10 0.10
SALICYLIC ACID SAB
Sodium
SODIUM BENZOATE benzoate 0.20 0.20 0.20
COLUMNAR
DISODIUM EDTA EDTA-2NA 0.20 0.20 0.20
A2 TITANIUM DIOXIDE
Selected A-
0.80 0.80 0.80
HRC
! ;
! :
81 DIMETHICONE
ISOHEXADECAN E
CAPRYLIC/CAPRIC
TRIGLYCERIDE
TITANIUM DIOXIDE
(and) DISODIUM
STEAROYL
GLUTAMATE (and)
ALUMINUM
HYDROXIDE
CAPRYL YL GLYCOL
TOCOPHERYL
ACETATE
SODIUM
82
ACRYLOYLDIMETHYL
TAURATENP
CROSSPOLYMER
SODIUM
ACRYLATE/SODIUM
ACRYLOYLDIMETHYL
c TAURATE
COPOLYMER (and)
ISOHEXADECANE
(and) POLYSORBATE
80
AMMONIUM
D POLYACRYLOYLDIME
THYLTAURATE
DIMETHICONENINYL
D DIMETHICONE
CROSSPOLYMER
E PHENOXYETHANOL
CITRUS LIMON
F (LEMON) FRUIT
EXTRACT
BIFIDA FERMENT
LYSATE
HYDROLYZED SOY
PROTEIN
ASCORBYL
GLUCOSIDE
TRIETHANOLAMINE
WATER
G SILICA
H TALC
I FRAGRANCE
14
Belsyldm 5+
Arlamol HD
WLFARESTE
R MCT7030
NAI-TAO-
77891
Dermosoft
Octiol
DL-ALPHA
TOCOPHERY
LACETATE
(0420085)
Aristoflex
AVS®
Simulgel EG®
HOSTACERIN
AMPS®(by
Lubrizol).
Dow Corning
9506 Powder
Sepicide LD
Secrets DE
Citron
Repair
complexCLR
PF
Phytokine
Hydrolyte 5
REFA0092
AA2G
Triethanolamin
e 99.0% CR C
7
Aqua
Sunsphere H
51
Luzenac
pharma M
Night Rescue
Mod 1
4.00
2.00
2.00
0.20
0.20
0.10
1
0.70
-
3
0.70
0.01
0.01
0.01
0.20
0.25
10.00
0.20
1.00
0.30
4.00
2.00
2.00
0.20
0.20
0.10
-
0.70
1
3
0.70
0.01
0.01
0.01
0.20
0.25
10.00
0.20
1.00
0.30
4.00
2.00
2.00
0.20
0.20
0.10
2
-
-
3
.
I I
i'
I'
i-:
I
I
15
The process for preparing formulas C to E is as described in example 1.
The stability of formulas A to E was measured according to the following protocol:
Formulas A to E were maintained during two months under the following conditions:
5 • At room temperature,
10
15
20
• In a chamber at 37°C,
• In a chamber at 45°C, and
• In a chamber at 4°C.
The organoleptic and physicochemical controls (including appearance, color, odor, pH
'ilnd viscosity) were conducted.
The results are as follows:
Formula c D E B A
(comparative) (comparative) (comparative) (invention) (invention)
Stability Emulsion not Emulsion not Emulsion not Emulsion is Emulsion is
results stable stable stable stable stable
It is observed from these results that the compositions of the present invention are stable
under normal storage conditions.
To the contrary, comparative formulas C to E are not stable.
Example 3: Instrumental test regarding skin color and skin hydration
The objective of this test is to understand the instant and long lasting fairness and
hydration effect of formula A using Chromasphere and Corneometer to compare the
efficacy with yogurt (BioKul Yogurt).
An instrumental evaluation was carried out on 24 healthy female subjects with fair and
25 medium-yellow skin tone (50:50) having dry skin (corneometer readings on forearm < 30)
using Chromasphere and Corneometer.
The product was applied in randomization pattern using split face design for its effects on
skin color. Also, the product was applied to forearm using a randomization for its effects
on skin hydration.
30 The amounts of product were the following:
Half face:
Formula A = 0.2g/half face
16
BioKul Yogurt= 0.5g/halfface
Forearm:
Formula A = 2mg/cm2 per site
5 BioKul Yogurt= 5mg/cm2 per site
10
The time points at which measurements were taken are:
Chromasphere : TO, T1 Om in, T1 hr, T 4hr & T7.5hr
Corneometer: TO, T1 hr, T4hr & T7.5hr
The study protocol was as follows :
1. Cleansing - Models wash face and forearm as per standard cleansing gesture with
standard cleanser
2. Acclimatization - 30 minutes waiting in temperature and humidity controlled waiting
15 area (Temperature: 21±1°C; Humidity: 50±5%)
3. TO measurements - Images taken on Orion Table & Chromasphere. Hydration
readings on forearm
4. Product Application - By expert applicator as per randomization for half face and
forearm application
20 For Yogurt application, the following procedure would be followed: apply yogurt (dosage
0.5g/half face & 5mg/cm2 per site on forearm), then 10min wait, then water wash, then
half face wash with cleanser.
Post application and cleansing of yogurt, formula A will be applied on the remaining half
face at a dosage of 0.2g/half face and 2mg/cm2 per site on forearm.
25 5. Waiting - 1 Ominutes waiting after application of product
6. T-imm measurements- Images taken on Orion Table & Chromasphere
7. Waiting- 1 hr waiting under controlled conditions
8. T1 hr measurements - Images taken on Orion Table & Chromasphere. Hydration
readings on forearm
30 9. Waiting - 3 hrs waiting under controlled conditions
35
10. T4hr measurements -Images taken on Orion Table & Chromasphere
11. Waiting - 4 hrs waiting under controlled conditions
12. T7.5HR measurements - Images taken on Orion Table & Chromasphere. Hydration
readings on forearm
The results are the following :
17
SSj indicates that Treatment 1 shows significantly higher values of that parameter as
5 compared to Treatment 2.
SS~ indicates that Treatment 1 shows significantly lower values of that parameter as
compared to Treatment 2.
Untreated
Yoghurt
Untreated
Yoghurt
A VS SS j ss i
10 NS<-+ indicates no significant difference between Treatment1 and Treatment2.
SSj indicates that Treatment 1 shows significantly higher values of that parameter as
compared to Treatment 2.
Conclusion: The overnight usage of formula A shows better efficacy as compared to
15 yogurt for skin hydration.
Example 4: Hydration test with formula A
18
The objective of this study was to determine the hydration effect of formula A.
All the subjects (24) were acclimatized to the required environmental conditions.
5 Instrumental evaluation by Corneometer for all the subjects was taken (TO), followed by
application of formula A. Post application, instrumental evaluation for all the subjects was
done at T-1 (30 min post application), T-4 hours and T-8 hours.
The further observation was on Day 1 at 24 hrs (T-24) wherein instrumental evaluation for
all the subjects was noted. At TO and T-8 hours D-Squame tape application was
10 performed on 12 selected subjects.
Formula A was applied on all the subjects. Out of 24 subjects, all the subjects followed the
study procedures and no discomfort was observed to any of the subject.
Moisture content on !eft and right volar forearm were measured using Corneometer® MPA
15 6 at pre product application, 30 min, 4 hours, 8 hours and after 24 hours of product usage.
Corneometer Readings:
The moisture content on all the target sites of volar forearm were measured using
Corneometer before application (0 min) (TO) and post application at 30min (T-1), 4 hours
20 (T-4), 8 hours (T-8) and after 24 hours (T-24) of product usage. Mean values for all
subjects were used for the analysis.
The results are as follows:
Hydration T-1 T-4 T-8 T-24
% evolution of +57.8% +22.4% +19.7% +13.6%
treated area
versus
baseline (TO)
% evolution of +14% +0.4% +2.2% +5.6%
untreated area
versus
baseline (TO)
25 When compared to Baseline, formula A has shown a statistically significant improvement
in moisture content levels at all time-points.
19
In view of the results, a significant moisturizing effect of formula A is observed at 30 min, 4
hours, 8 hours and 24 hours after the application, compared to the initial values and to an
untreated area.
CLAIMS
1. Composition, preferably a cosmetic composition, comprising:
- a fatty phase dispersed in a continuous aqueous phase, said continuous aqueous
5 phase comprising at least three polyols, and
- at least three crosslinked or non-crosslinked copolymers comprising 2-acrylamido
2-methyl propane sulfonic acid units.
2. Composition of claim 1, wherein the crosslinked or non-crosslinked
10 copolymers comprising 2-acrylamido 2-methyl propane sulfonic acid units are partially or
completely neutralized with an inorganic base, such as sodium hydroxide, potassium
hydroxide or aqueous ammonia, or an organic base such as mono-, di- or triethanolamine,
an aminomethylpropanediol, N-methylglucamine or basic amino acids such as arginine
and lysine, and mixtures of these compounds.
15
3. Composition of claim 1 or 2, wherein, when the copolymers are
crosslinked, the crosslinking agents are chosen from compounds with an olefinic
polyunsaturation commonly used for crosslinking polymers obtained by radical
polymerization, preferably from divinylbenzene, diallyl ether, dipropylene glycol diallyl
20 ether, polyglycol diallyl ethers, triethylene glycol divinyl ether, hydroquinone diallyl ether,
ethylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, trimethylolpropane
triacrylate, methylenebisacrylamide, methylenebismethacrylamide, triallylamine, triallyl
cyanurate, diallyl maleate, tetraallylethylenediamine, tetraallyloxyethane,
trimethylolpropane diallyl ether, allyl (meth)acrylate, allyl ethers of alcohols of the sugar
25 series, or other allyl or vinyl ethers of polyfunctional alcohols, and also allyl esters of
phosphoric acid derivatives and/or vinylphosphonic acid derivatives, or mixtures of these
compounds.
4. Composition of any one of claims 1 to 3, wherein the 2-acrylamido-2-
30 methylpropanesulphonic acid copolymers comprise units of general formula (1):
(I)
21
in which X+ denotes a proton, an alkali metal cation, an alkaline earth metal cation
or the ammonium ion, it being possible for no more than 10 mol % of the X+ cations to be
H+ protons;
and crosslinking units originating from at least one monomer having at least two
5 olefinic double bonds.
5. Composition of any one of claims 1 to 4, wherein the 2-acrylamido-2-
methylpropanesulphonic acid (AMPS) copolymers are chosen from:
- crosslinked copolymers of acrylamide or methacrylamide and of 2-acrylamido-2-
1 0 methyl propane sulfonate;
15
20
25
30
- copolymers of AMPS and vinylpyrrolidone or vinylformamide; and
- copolymers of AMPS and sodium acrylate.
6. Composition of any one of claims 1. to 5, wherein the 2-acrylamido-2-
methylpropanesulphonic acid copolymers are present in amounts of active material
ranging from 0.01 to 20% by weight, more preferably from 0.1 to 10% by weight, even
more preferably from 0.5 to 5% by weight and more particularly from 0.8 to 2% by weight
relative to the total weight of the composition.
7. Composition of any one of claims 1 to 6, which comprises at least one
AMPS copolymer chosen from copolymers of AMPS and vinylpyrrolidone or
vinylformamide, preferably vinylpyrrolidone.
8. Composition of any one of claims 1 to 7, wherein the 2-acrylamido-2-
methylpropanesulphonic acid copolymers are a mixture of:
- at least one crosslinked copolymer of acrylamide or methacrylamide and of AMPS;
- at least one copolymer of AMPS and vinylpyrrolidone or vinylformamide; and
- at least one copolymer of AMPS and sodium acrylate.
9. Composition of any one of claims 1 to 8, wherein the continuous
aqueous phase is present in an amount ranging from 10% to 99% by weight, more
preferably from 20% to 95% by weight, and even more preferably from 50% to 90% by
weight of the total weight of the composition.
35 10. Composition of any one of claims 1 to 9, which comprises water and a
mixture of glycerol, butylene glycol and pentylene glycol.
i
'I
! ·ii
il
il
jl
d
]!
!I
I
22
11. Composition of any one of claims 1 to 10, wherein the dispers~d fatty
phase is present in an amount ranging from 1% to 60% by weight, preferably from 3% to
40% by weight, more preferably from 5% to 30% by weight, more preferably from 5% to
5 20% by weight, relative to the total weight of the composition, and preferably comprises at
least one volatile or non-volatile, hydrocarbonated, silicone or fluorinated, oil.
10
15
-
12. Composition of any one of claims 1 to 11, which comprises:
- from 70% to 90% of a mixture of water, glycerol, butylene glycol and pentylene
glycol;
-from 5% to 15% of at least one oil;
- from 0.1% to 1% of at least one crosslinked copolymer of acrylamide or
methacrylamide and of AMPS;
- from 0.1% to 1.5% of at least one copolymer of AMPS and vinylpyrrolidone or
vinylformamide; and
- from 0.1% to 1% of at least one copolymer of AMPS and sodium acrylate.
13. Composition of any one of claims 1 to 12, which comprises less than 2%
by weight, preferably less than 1% by weight, more preferably less than 0.5% by weight of
20 the total composition, of emulsifiers, more preferably is devoid of emulsifiers.
25
14. A method for caring for the skin, comprising the application to the skin of
the composition of any one of claims 1 to 13.
15. A process for preparing a composition of any one of claims 1 to 13,
comprising the steps of:
a) mixing at least three glycols and at least one crosslinked or non-crosslinked
copolymer comprising 2-acrylamido 2-methyl propane sulfonic acid units, in order
to obtain an aqueous phase, at room temperature; ·
30 b) mixing fatty components and at least one crosslinked or non-crosslinked
copolymer comprising 2-acrylamido 2-methyl propane sulfonic acid units, in order
to obtain a fatty phase, at room temperature; and
c) introducing the fatty phase obtained in step b) into the aqueous phase obtained in
step a), in order to obtain an oil-in-water emulsion.
| # | Name | Date |
|---|---|---|
| 1 | Power of Attorney [10-03-2017(online)].pdf | 2017-03-10 |
| 2 | Form 5 [10-03-2017(online)].pdf | 2017-03-10 |
| 3 | Form 3 [10-03-2017(online)].pdf | 2017-03-10 |
| 4 | Description(Complete) [10-03-2017(online)].pdf_206.pdf | 2017-03-10 |
| 5 | Description(Complete) [10-03-2017(online)].pdf | 2017-03-10 |
| 6 | 201711008478-REQUEST FOR CERTIFIED COPY [14-02-2018(online)].pdf | 2018-02-14 |
| 7 | 201711008478-PETITION UNDER RULE 137 [31-07-2018(online)].pdf | 2018-07-31 |
| 8 | 201711008478-FORM-8 [31-07-2018(online)].pdf | 2018-07-31 |
| 9 | 201711008478-Proof of Right (MANDATORY) [01-08-2018(online)].pdf | 2018-08-01 |
| 10 | 201711008478-Power of Attorney-010818.pdf | 2018-08-03 |
| 11 | 201711008478-OTHERS-010818.pdf | 2018-08-03 |
| 12 | 201711008478-OTHERS-010818-.pdf | 2018-08-03 |
| 13 | 201711008478-Correspondence-010818.pdf | 2018-08-03 |
| 14 | 201711008478-Correspondence-010818-.pdf | 2018-08-03 |
| 15 | 201711008478-FORM 3 [26-10-2018(online)].pdf | 2018-10-26 |
| 16 | 201711008478-FORM 18 [10-02-2021(online)].pdf | 2021-02-10 |
| 17 | 201711008478-FER.pdf | 2021-10-17 |
| 18 | 201711008478-PETITION UNDER RULE 137 [05-01-2022(online)].pdf | 2022-01-05 |
| 19 | 201711008478-OTHERS [05-01-2022(online)].pdf | 2022-01-05 |
| 20 | 201711008478-FER_SER_REPLY [05-01-2022(online)].pdf | 2022-01-05 |
| 21 | 201711008478-COMPLETE SPECIFICATION [05-01-2022(online)].pdf | 2022-01-05 |
| 22 | 201711008478-CLAIMS [05-01-2022(online)].pdf | 2022-01-05 |
| 23 | 201711008478-US(14)-HearingNotice-(HearingDate-02-11-2022).pdf | 2022-09-28 |
| 24 | 201711008478-FORM-26 [28-10-2022(online)].pdf | 2022-10-28 |
| 25 | 201711008478-Correspondence to notify the Controller [28-10-2022(online)].pdf | 2022-10-28 |
| 26 | 201711008478-Written submissions and relevant documents [16-11-2022(online)].pdf | 2022-11-16 |
| 27 | 201711008478-Response to office action [18-11-2022(online)].pdf | 2022-11-18 |
| 28 | 201711008478-PatentCertificate13-02-2023.pdf | 2023-02-13 |
| 29 | 201711008478-IntimationOfGrant13-02-2023.pdf | 2023-02-13 |
| 1 | SearchstrategyE_20-09-2021.pdf |