Title of Invention

A TRANSPARENT AND STORAGE STABLE LIQUID COSMETIC COMPOSITION

Abstract Abstract The present invention relates to transparent, storage stable, pourable liquid cosmetic compositions that contain a substantial amount of water and oil for topical application to skin and hair. In particular, the invention relates to transparent, storage stable, pourable liquid cosmetic compositions having a viscosity of from 10 cP to 200 cP comprising at least 10% water, one or more emulsifiers comprising at least 80% lecithin and co-emulsifier, wherein said oil is the continuous phase. 18
Full Text FORM -2
THE PATENTS ACT, 1970
(39 of 1970)
COMPLETE SPECIFICATION
(See Section 10)
COSMETIC COMPOSITION
HINDUSTAN LEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India

The following specification particularly describes the nature of the invention and the manner in which it is to be performed.




TECHNICAL FIELD
The present invention relates to transparent, storage stable, pourable liquid cosmetic compositions that contain a substantial amount of water and oil for topical application to skin and hair. In particular, the invention relates to transparent, storage stable, pourable liquid cosmetic compositions having a viscosity of from 10 cP to 200 cP.
BACKGROUND AND PRIOR ART
In many countries, oiling of hair (primarily with vegetable oils) is a common practice. It is also a common practice to apply the oil onto skin. Oil helps in the styling of hair. Oil is also believed to have nutritive and beneficial effects on skin and hair.
Transparency is an important cue for non-adulteration of cosmetic oil and is a consumer desired attribute. Oils containing benefit agents are also desired by consumers. However, many benefit agents (such as vitamins, colorants and proteins) are water soluble or hydrophilic in nature and cannot be incorporated in oils since the oil loses its clarity and transparency.
It would be thus advantageous to provide for liquid cosmetic compositions which appear like oil, which can be easily applied to skin and/or hair and which offer the benefits of oils as well as benefits due to water-soluble functional ingredients. One of the ways of achieving this is by incorporating water in the oil. It is required that the water should be the dispersed phase in the oil in order to retain the advantageous properties of oil. Additionally, it will then be possible to incorporate water soluble benefit agents in these liquid cosmetic compositions.
However, it is required that the liquid cosmetic composition be transparent in nature as transparency in hair and skin oils is perceived as a cue for purity by consumers. Further, the compositions are required to be storage stable as


compositions comprising water and oil are known to phase separate on storage.
Transparent compositions where water is dispersed in a continuous oil phase are known in the prior art.
Thus,
-WO 9426234 (IBAH Inc.) describes water -in- oil microemulsions containing up to 5 % by wt. water for use as lip balm. The oil is preferably triglyceride and the nonionic surfactant used to obtain the microemulsion is chosen from methyl glucoside derivatives, polyglycerol esters, triglycerol monooleate, monoglycerides and ethoxylated derivatives.
JP 2015015A2 (Kanebo Ltd.) discloses a liquid oily cosmetic having transparency, excellent appearance, storage stability and providing moisture retention, flexibility and moist feeling after application. The formulation contains 3-6 % water and contains a hydrophilic nonionic emulsifier, i.e., polyoxyethylene sorbitan monooleate.
WO 9302665 (SmithKline Beecham Corporation) relates to a stable, water-in-oil microemulsion that comprises a lipophilic phase, a low HLB (hydrophilic lipophilic balance) surfactant, a high HLB surfactant, an aqueous phase and a water soluble therapeutic agent. The invention provides for microemulsions that have a water content of less than 10%. Further the microemulsion does not use lecithin as a surfactant.
WO 0032153 (University of Nottingham) describes fragrance releasing compositions comprising water-in-oil microemulsion droplets wherein the droplets have low water activity and contain the fragrance. The microemulsions disclosed have about 3% water and more than 80% oil. The compositions may include co-surfactants like short chain alcohols. Lecithin is disclosed as a surfactant.


US 6004580 (Leiras Oy) deals with pharmaceutical oil-in-water or bi-continuous microemulsions comprising oil, water, a surfactapt and a drug. Up to 10% oil is used to form the microemulsions. Lecithin is used as a surfactant to form these microemulsions. The microemulsions are in the form of gels.
US5298240 (Wella) pertains to a hair care composition in the form of a microemulsion gel containing a) from 5 to 20 percent by weight of nonionic surfactants with an HLB-value of from 5 to 12 or mixtures of the nonionic surfactants, the mixtures having HLB-values of from 6 to 10; b) from 5 to 20 percent by weight of at least one oil; c) from 0.5 to 10 percent by weight of at least one cationic surfactant; and d) from 50 to 89.5 percent by weight water. The said microemulsion is an oil-in-water microemulsion.
Thus, the prior art does not disclose liquid cosmetic compositions comprising oil and more than 10% water. The likely reason for this is that increasing the amount of water would result in non-transparent compositions with poor storage stability.
The present inventors now disclose transparent and storage stable liquid cosmetic compositions comprising oil, at least 10% water, one or more emulsifiers comprising at least 80% lecithin and a co-emulsifier, wherein the oil is the continuous phase. The liquid cosmetic compositions of the invention retain many of the advantageous properties of hair or skin oil, and are capable of being topically applied to skin and/or hair. Both oil and water soluble benefit agents can be incorporated in the liquid cosmetic composition of the invention. The liquid cosmetic compositions are also cooling to the touch.
OBJECTS OF THE INVENTION
!t is an object of the invention to provide for a transparent, storage stable, pourable liquid cosmetic composition comprising oil and at least 10% water that shows the attributes of a hair or skin oil.


It is a further object of the invention to provide for a transparent, storage stable, pourable liquid cosmetic composition comprising oil and at least 10% water that is cooling to the touch.
It is another object of the invention to provide for a transparent, storage stable liquid cosmetic composition comprising oil and at least 10% water that will uniformly coat the surface of the hair.
SUMMARY OF THE INVENTION
The present invention is directed towards transparent and storage stable, pourable liquid cosmetic compositions comprising a suitable amount of oil, at least 10% water, one or more emulsifiers comprising at least 80%o lecithin and a co-emulsifier, wherein the oil is the continuous phase. The liquid cosmetic composition has a viscosity in the range of 10 to 200 cP, The liquid cosmetic composition shows superior or similar properties to hair oils. Further, it gives a good appearance to the hair and is cooling to the touch. The liquid cosmetic compositions can be topically applied to skin and/or hair and are particularly suitable for oiling and styling of hair. The liquid cosmetic compositions also spread better on hair as compared to hair oil. A range of benefit agents can be solubilised either in the oil or water phase and delivered to the hair.
DEFINITION OF THE INVENTION
According to the first aspect of the invention, there is provided a transparent
and storage stable liquid cosmetic composition having viscosity in the range
of 10 to 200 cP comprising oil, at least 10% water, one or more emulsifiers
comprising at least 80% lecithin and co-emulsifier, wherein said oil is the
continuous phase.
According to a preferred aspect of the invention, there is provided a
transparent, storage stable liquid cosmetic composition comprising:
30- 75% oil
10-25% water
5-40% of one or more emulsifiers comprising at least 80% lecithin
said compositions having a viscosity of from 10 to 200 cP and
1-15% co-emulsifier


According to the second aspect of the invention, there is provided a process to prepare the transparent, storage stable composition comprising the steps
of:
i(a) Mixing of oil phase and the emulsifier to.form a uniform mixture.
(b) Addition of co-emulsifiers and water to (a)
DETAILED DESCRIPTION OF THE INVENTION
All parts herein are by weight unless otherwise described.
THE TRANSPARENT. STORAGE STABLE COMPOSITION
The transparent, pourable, storage stable liquid cosmetic composition of the invention comprises:
30-75% oil
10-25% water
5-40% of one or more emulsifiers comprising at least 80% lecithin
1-15% co-emulsifier
said compositions are having a viscosity of from 10 to 200 cP.
Preferably, the transparent, storage stable composition of the invention comprises:
30-60% oil
10-25% water
5-37% of one or more emulsifiers comprising at least 80% lecithin.
5-12% co-emulsifier
said compositions having a viscosity of from 20 to 85 cP.


More preferably, the transparent, storage stable composition of the invention
comprises:
50-60% oil
15-25% water
5-37% of one or more emulsifiers of which at least 95% is liquid lecithin
comprising at least 33 % by wt. soybean oil and at least 66 % by wt. actives
such that the actives mainly constitute di-n-alkyl phosphatidylcholine, di-n-
alkyl phosphatidyl ethanolamine, di-n-alkyl phosphatidyl inositol and
phosphatidic acid.
7-12% co-emulsifier
said compositions having a viscosity of from 30 to 50 cP.
The transparent, storage stable liquid cosmetic composition of the invention comprises oil and water, wherein the oil is the continuous phase. The water dispersed in the oil phase has a droplet size less than 100 nm thus providing for transparency.
The transparent, storage stable liquid cosmetic composition of the invention is suitable for use as hair oil.
THE OIL PHASE
The oil phase can be chosen from paraffin oil or vegetable oils. Vegetable oils are typically long chain triglycerides. Triglycerides with alkyl chain lengths in the range of carbon number 6-22 are particularly preferred for the compositions of the invention. Examples of vegetable oils suitable for the invention include coconut oil, olive oil, sesame oil, groundnut oil, sunflower oil; safflower oil, castor oil, and soybean oil or their mixtures thereof. Unsaturated and hydrogenated oils are also encompassed by the invention.
Both linear and randomly branched chain hydrocarbons are suitable
for the invention. Particularly preferred hydrocarbons are randomly branched chain paraffin oils.


It is also possible to use a mixture of hydrocarbons and vegetable oils as the oil phase.
THE EMULSIFIER
It is possible to use one or more emulsifiers to make the liquid cosmetic composition of the invention provided that at least 80% of it is lecithin. The lecithin is preferably an extract of soybean comprising at least 33 % by wt. soybean oil and at least 66 % by wt. actives. Preferably, the actives comprise di-n-alkyl phosphatidylcholine, di-n-alkyl phosphatidyl ethanolamine, di-n-alkyl phosphatidyl inositol and phosphatidic acid. The carbon chain length of the aforementioned actives varies from
Other emulsifiers may optionally be present provided the amount does not exceed 20%. Examples include glycerol monooleate, sorbitan monooleate, sorbitan monolaurate, Alkyl polyglucosides (Glucopone 215, Glucopone 600, Glucopone 650), Sodium bis(2-ethylhexyl sulfosuccinate)(AOT) and alcohol ethoxylates
THE CO-EMULSIFIER
The co-emulsifiers can be chosen from alpha hydroxy acids and their salts, short-chain alcohols, alkane 1,2 diols or their mixtures
thereof. Lactic acid or sodium lactate is a preferred co-emulsifier among alpha hydroxy acids and their salts. An especially preferred short chain alcohol is isopropyl alcohol. Octane-1,2 diol is a preferred alkane 1-2 diol co-emulsifier.
OPTIONAL INGREDIENTS
It is also possible to incorporate benefit agents and other additives in the transparent, storage stable liquid cosmetic composition provided the stability and transparency of the transparent, storage stable composition is retained.



Examples of additives include hair styling polymers; water-soluble colorants; anti-dandruff agents; vitamins; proteins; extracts from plants such as Ocimum Sanctum (tulsi), Hibiscus rosa-sinensis, Embelica officinalis (amla) etc.
Hair styling polymers suitable for the invention include, Luviscol™, polyethyleneimine, quarternized hydroxyethyl cellulose, polypeptides amongst others.
Anti-dandruff agents suitable for incorporation are salicylic acid, zinc pyrithione etc.
In addition to oil soluble vitamins, water-soluble vitamins like Vitamin B, Vitamin C can be advantageously included in the hair oil.
METHOD OF MAKING THE TRANSPARENT. STORAGE STABLE COMPOSITION
The method of the making transparent, storage stable composition is as known in the conventional art. Oil (e.g., coconut oil, paraffin oils etc.) and emulsifier are first mixed to form a solution/ homogeneous mixture. The co-emulsifier and water are subsequently added to the solution/homogeneous mixture to obtain the transparent, storage stable liquid cosmetic composition that is a single phase. The mixing can be carried out by conventional means.
If present, water and/or oil-insoluble impurities that reduce the clarity of the composition, are separated by centrifugal action or by filtration.
Reference is made in the examples to accompanying figures.


EXAMPLES
Example 1
Phase diagrams were determined to obtain water-in-oil transparent, storage stable liquid cosmetic compositions containing coconut oil, water, liquid soybean lecithin and isopropanol (IPA).
Figure 1 represents the phase diagram for (Coconut Oil-Water-liquid soybean lecithin-lsopropanol) at 25 °C wherein the oil to water ratio is 1:1. The figure provides the single-phase (transparent) region and the ratio of soybean lecithin liquid/lPA needed to obtain the transparent, storage stable state.
Using the ratio of soybean lecithin liquid/lPA as obtained from Figure 1, a ternary phase diagram of water, coconut oil and soybean lecithin liquid/lPA (ratio: 78/22) was obtained and is given in Figure 2. The formulation of the transparent, storage stable liquid compositions of the invention forming a single phase are obtained from Figure 2 (unshaded region). In Figure 2, E and co-E stand for emulsifier and co-emutsifier respectively.
Figure 3 is a phase diagram of a (paraffin oil/water/soybean lecithin liquid/1-propanol) system. The paraffin oil (LLPO) is a randomly branched
hydrocarbon. The (0,0) point of the graph represents LLPO:(Water+1-propanol) = 1:1. The single phase, transparent liquid cosmetic compositions are obtained from the unshaded region of the phase diagram. The concentration of 1-propanol in water is given in weight fraction.
The phase diagrams (Figures 1, 2 and 3) clearly indicate that single-phase, transparent, storage stable liquid cosmetic compositions of suitable characteristics are only formed within the range and composition defined by the invention.
The formulation details of transparent, storage stable liquid cosmetic compositions within and outside the invention are presented in Table 1 and 2.




Table 1:

Example Oil Emulsifier mix *Co-emulsifier
A Coconut oil Sorbitan Oleate Isopropanol
B Coconut Oil Fynol GO1 M Isopropanol
C Coconut Oil Sodium dioctyl Sulfosuccinate (AQT) Isopropanol
-
D Coconut Oil Sorbitan Oleate ._ Ethanol
E Coconut Oil Liquid soybean lecithin(General Foods)(33.3%) Fynol GO™ (66.7%)
1 Coconut Oil Liquid soybean lecithin(General Foods) Isopropanol
2 Coconut Oil Liquid soybean lecithin(General Foods) Isopropanol
3 Coconut Oil Liquid soybean lecithin(General Foods) Isopropanol
4 Coconut oil Liquid soybean lecithin(General Foods) 1-propanol: 1-Butanol
5 Paraffin (LLPO) Liquid soybean lecithin(General Foods) Isopropanol
Table 2:

Example Oil (%) Water
(%) Emulsifier
mix (%) Co-emulsifier
(%) Single-Phase Composition
A 33 15 40 12 No
B 33 15 40 12 No
C 33 15 40 12 No
D 38.6 38.6 19 3.8 No
E 20 20 60 - No
1 54.7 10 27.5 7.8 Yes
2 42.7 15 33 9.3 Yes
3 31.3 20.4 37.3 10.9 Yes
4 38 22 24 16 Yes
5 31.5 21.5 37 10 Yes


The liquid cosmetic compositions of the invention are transparent in the temperature region of 5 to 60 °C. However compositions containing coconut oil (examples 1-4) are opaque at temperatures of 24 °C and below due to the inherent property of coconut oil. On heating to a temperature >24 °C, the liquid cosmetic compositions are transparent up to 60 °C.
Transparency
The transparency of the liquid cosmetic compositions of Examples A-E, Examples 1-5 as well as coconut oil and LLPO were determined. The sample was taken in a quartz cuvette of 1 cm path length. Light transmittance (%T) was measured at 650 nm using a Carry 50 UV-Visible Spectrometer. The wavelength of 650 nm was chosen for measurement as absorption bands due to lecithin were observed at wavelengths less than 600 nm. The sample temperature was 25 degrees centigrade. The higher the percent transmittance, the greater the transparency of the liquid composition. The results are presented in Table 3.
Table 3

Example % Transmittance (650 nm)
A 0.03
B 0.04
C 3.85
D 0.003
uj 0.001
1 78.8
2 69
3 65.2
4 70.8
5 66
Coconut Oil 67
LLPO 86.7


The data presented in Table 3 shows that the examples outside the invention provide for opaque liquid cosmetic compositions. Examples relating to the invention provide for transparent liquid cosmetic compositions with a transparency similar to that of pure oils like coconut oil or paraffin.
Spreadability
Experiments were performed to determine the spreadabiiity of the transparent, storage stable liquid cosmetic compositions on hair fibres. 10 to 20 microlitres of coconut oil and the composition of Example 4 was brought in contact with a single strand of hair fibre, tied on to a microscope stage.
The transferred oil film immediately formed pearl-like droplets on the hair fibre. Equilibrium contact angle of the droplets was measured on a Zeiss Microscope.
Equilibrium contact angles for the pure coconut oil and Example 4 were found to be 20 and 10 degree respectively. Lower contact angle for the composition of the invention indicates its better spreadabiiity on hair fibre as compared to conventional hair oil.
Thus the present invention provides for a transparent, storage stable liquid cosmetic composition comprising a large amount of water and oil and having better spreadabiiity. The compositions of the invention are suitable for use as hair oil and show attributes similar or superior to conventional hair oils.


We claim:
1. A transparent and storage stable liquid cosmetic composition having viscosity
in the range of 10 to 200 cP comprising:
i. 30-75% oil; ii. 10-25%water;
iii. 5-40% of one or more emulsifiers comprising at least 80% lecithin; and iv. 1-15% co-emulsifier, wherein said oil is the continuous phase.
2. A transparent and storage stable liquid cosmetic composition as claimed in
claim 1 having a viscosity of from 21 to 85 cP comprising:
i. 30-60% oil;
ii. 10-25% water;
iii. 5-37% of one or more emulsifiers comprising at least 80% lecithin; and
iv. 5-12% co-emulsifier.
3. A transparent and storage stable liquid cosmetic composition as claimed in
anyone of claims 1 to 2 having a viscosity of from 30 to 50 cP comprising:
i. 50-60% oil;
ii. 15-25% water;
iii. 5-37% of one or more emulsifiers of which at least 95% is liquid lecithin comprising at least 33% by wt. soybean oil and at least 66% by wt. actives such that the actives mainly constitute di-n-alkyl phosphatidylcholine, di-n-alkyl phosphatidyl ethanotamine, di-n-alkyl phosphatidyl inositol and phosphatidic acid; and
iv. 7-12% co-emulsifier.


4. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 3 wherein the water dispersed in the oil phase has a droplet size (ess than 100 nm for required transparency.
5. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 4 wherein the said oil phase is selected from paraffin oil, vegetable oils, unsaturated and hydrogenated oils.
6. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 5 wherein the vegetable oils comprise long chain triglycerides preferably with alkyl chain lengths in the range of carbon number 6-22.
7. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 6 wherein the oil phase comprise both linear and randomly branched chain hydrocarbons preferably hydrlcarbons with randomly branched chain paraffin oils.
8. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 7 wherein said lecithin in said emulsifier comprise an extract of soybean comprising at least 33% by wt. soybean oil and at least 66% by wt. actives.
9. A transparent and storage stable liquid cosmetic composition as claimed in claim 8 wherein the actives comprise di-n-alkyl phosphatidylcholine, di-n-alkyl phosphatidyl ethanolamine, di-n-alkyl phosphatidyl inositol and phosphatidic acid, the carbon chain length of the aforementioned actives varies from to



10.A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 8 to 9 comprising optionally other emulsifiers not exceeding
20%.
11. A transparent and storage stable liquid cosmetic composition as claimed in claim 10 wherein the said other emulsifiers are selected from glycerol monooleate, sorbitan monooleate, sorbitan monolaurate, Alkyl polyglucosides Sodium bis (2-ethylhexyl sulfosuccinate) and alcohol ethoxylates
12. A transparent and storage stable liquid cosmetic composition as claimed in anyone of claims 1 to 11 wherein said co-emulsifiers are selected from alpha hydroxy acids and their salts, short-chain (C2-C6) alcohols, alkane (C8-C12) 1,2 diols or mixtures thereof preferably lactic acid or sodium lactate co-emulsifier among alpha hydroxy acids and their salts more preferably short chain alcohol isopropyl alcohol and Octane-1,2 diol as preferred alkane 1-2 diol co-emulsifier.
13.A process for preparing the transparent, storage stable composition as claimed in anyone of claims 1 to 12 comprising the steps of:
a) mixing of 30-75% oil phase and 5-40% of one or more emulsifiers comprising at least 80% lecithin; to form a uniform mixture;
b) addition of 1-15% of co-emulsufiers and 10-25% of water to a).
14. A process as claimed in claim 13 wherein water and/or oil-insoluble impurities if any are separated by centrifugal action or by filtration.

Documents:

1099-mum-2001-abstract.doc

1099-mum-2001-abstract.pdf

1099-mum-2001-cancelled pages(20-11-2001).pdf

1099-mum-2001-claims(cancelled).pdf

1099-mum-2001-claims.doc

1099-mum-2001-claims.pdf

1099-mum-2001-correspondence 1(08-09-2004).pdf

1099-mum-2001-correspondence 2(08-02-2007).pdf

1099-MUM-2001-CORRESPONDENCE(8-2-2012).pdf

1099-mum-2001-correspondence(ipo)-(08-09-2004).pdf

1099-mum-2001-correspondence(ipo).pdf

1099-mum-2001-correspondence.pdf

1099-mum-2001-description(granted).doc

1099-mum-2001-description(granted).pdf

1099-mum-2001-drawing(20-11-2001).pdf

1099-mum-2001-drawing.pdf

1099-mum-2001-form 1(20-11-2001).pdf

1099-mum-2001-form 1.pdf

1099-mum-2001-form 18.pdf

1099-mum-2001-form 19(23-06-2003).pdf

1099-mum-2001-form 19.pdf

1099-mum-2001-form 2(granted)-(20-11-2001).pdf

1099-mum-2001-form 2(granted).doc

1099-mum-2001-form 2(granted).pdf

1099-mum-2001-form 2(provisional).pdf

1099-mum-2001-form 2(title page).pdf

1099-mum-2001-form 3(15-11-2002).pdf

1099-mum-2001-form 3.pdf

1099-mum-2001-form 5(15-11-2002).pdf

1099-mum-2001-form 5.pdf

1099-mum-2001-general power of attorney(27-01-2004).pdf

1099-mum-2001-patent of japan.pdf

1099-mum-2001-patent of japanese government.pdf

1099-mum-2001-power of attorney.pdf

abstract1.jpg


Patent Number 204581
Indian Patent Application Number 1099/MUM/2001
PG Journal Number 31/2008
Publication Date 01-Aug-2008
Grant Date 27-Feb-2007
Date of Filing 20-Nov-2001
Name of Patentee HINDUSTAN UNILEVER LIMITED
Applicant Address 165/166, BACKBAY RECLAMATION, MUMBAI
Inventors:
# Inventor's Name Inventor's Address
1 ROUT DEELEEP KUMAR B-212, NATASHA GOLF VIEW APARTMENT, NEW RING ROAD, DOMLUR, BANGALORE - 560 071,
2 NAIK VIJAY MUKUND, No. 800, 1'CROSS, 12 MAIN. INDLRANAGAR, HAL II STAGE. BANGALORE - 560 008,
3 SANYAL SAURAV, 720/6. C/O Y. NANJA REDDY, NANJA REDDY BUILDING, MUNNEKOLALA. MARATRIAHALLI POST, BANGALORE - 560 037,
PCT International Classification Number A 61 K 7/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA