Title of Invention

"A PROCSS FOR PREPARATION OF ANTIFUNGAL & ANTIDANDRUFF SHAMPOO COMPOSITION"

Abstract TRANSPARENT ANTIDANDRUFF SHAMPOOS Aqueous shampoo compositions whose washing base consists of an anionic surfactant and an amphoteric surfactant, in which some of the amphoteric agent consists of undecylenamidopropylbetaine, are described. This amphoteric principle gives these compositions effective antifungal properties against the action of Pityrosporum ovalae and constitutes a treatment for reducing the formation of dandruff.
Full Text The present invention relates to an aqueous shampoo
compositions which are useful in cosmetology, in particular shampoos and foaming gels, which are intended to care for the hair and/or the scalp, in particular to combat dandruff or to prevent its formation. The invention is directed towards shampoos whose washing base contains an amphoteric surfactant and an anionic surfactant, where appropriate supplemented with a thickener and/or a hair conditioner.
In shampoos whose washing base contains an anionic surfactant and an amphoteric surfactant, the washing function itself is based on the two components, but a foaming function is provided by the amphoteric surfactant. In very general terms, the amphoteric surfactant is an alkylbetaine, in particular a lauric-, coconut- or palm kernel-based alkylamidopropylbetaine. The mechanical elimination of dandruff, the causative agent of which is a fungus, Pityrosporum ovalae, is one of the expected results of shampooing, but it has also been sought to develop shampoos which combat or prevent the formation of dandruff. For this, use has been made of various antifungal agents.
Among the standard antifungal agents, mention may be made of:
- preserving agents whose fungal spectrum is oriented towards fungi and particularly yeasts, such as sorbic acid and dehydroacetic acid,
active agents listed as anti-yeast agents,
such as zinc pyrithione, piroctone-olamine and
clirabazole,
- a few surfactants derived from undecylenic
acid, in particular 4-sulpho-{2-[(l-oxo-10-
undecenyl)amino]ethyl}butanedioic ester, disodium
(RN=26650-05-5) (or disodium undecylenamido MEA sulphosuccinate, according to the CTFA name adopted in the International Cosmetic Ingredient Dictionary, 6th edition, by The Cosmetics, Toiletry and Fragrance Association, 1995), and N-(2-hydroxyethyl)undecenamide
(RN=20545-92-0 and 40839-40-5) (CTFA : undecylenamide MEA) .
However, some antifungal active principles among those most commonly used show cytotoxic potential in vitro. It is necessary to lower the working amounts thereof to below an acceptable cytotoxicity threshold, or even to combine them with molecules which protect the integrity of skin cells which are damaged or inflamed to a greater or lesser extent. These products have other drawbacks: for example, piroctone-olamine poses coloration problems in shampoos containing this active principle, zinc pyrithione is a water-insoluble powder which leads to opaque formulations that are unstable in light, climbazole is water-insoluble and requires the mandatory use of solvents (ethanol, benzyl alcohol).
As regards the undecylenic acid derivatives, some have already been cited for their antibacterial and antifungal activity, in particular the zinc salts of undecylenamido MEA sulphosuccinate (WO 97/18823 of 29.05.97 from Pierre Fabre; EP 23676 of 11.02.81 from Rewo) and of tricarboxylic acid which are derived from :he product of the Diels-Alder reaction between maleic anhydride and undecylenic acid (EP 71025 of 9.02.83 Erom Grillo Werke AG), as well as a number of esters (JP 08/053,326 of 27.02.96 from Kanebo; EP 28459 of L3.05.81 from Imperial Chemical Industries Ltd.). As examples, among the most common undecylenic acid derivatives are found N-(2-hydroxyethyl)undecenamide (CTFA : undecylenamide MEA) and 4-sulpho-{2-[(l-oxo-10-undecenyl)amino]ethyl}butanedioic ester, disodium (CTFA : disodium undecylenamido MEA sulphosuccinate), which are sold, respectively, under the trade names "Rewocid®U185 or Witcamide®6570" and "Rewocid®SB U185" by the company Witco. However, these derivatives are not amphoteric.
It has been discovered, unexpectedly, that in addition to the usual characteristics of betaines (co-surfactant, good foaming power, mild detergent), N-(carboxymethyl)-N,N-dimethyl-3-[(1-oxoundecenyl)amino]-1-propanaminium hydroxide (RN = 98510-75-9, neutral zwitterionic form) or CTFA : undecylenamidopropylbetaine
(Formula Removed)
has antifungal activity towards Pityrosporum ovalae and thus develops antidandruff efficacy which has never been cited to date. Consequently, it offers the very great advantage of being able to constitute an amphoteric component of a shampoo which itself has the desired antidandruff properties. This discovery is exploited in shampoos of the invention, which are essentially aqueous compositions of a washing base consisting of amphoteric surfactants and anionic surfactants and whose amphoteric surfactants do themselves - and this is the characteristic of the invention - partly consist of undecylenamidopropyl-betaine.
For the purposes of the invention, the term anionic surfactant is understood to refer to one or more compounds taken from the group formed of (C10 to C14)alkyl sulphates and (C10 to C14)alkyl ether sulphates. Lauryl ether sulphates are anionic surfactants used commonly by shampoo formulators.
For the purposes of the invention, the term amphoteric surfactant is understood to refer to the compounds chosen, alone or as a mixture, from alkyl amphocarboxyglycinates, alkyl amphocarboxypropionates, alkyl amphodiacetates, alkyl amphodipropionates, alkyl
amphoglycinates, alkyl amphopropionates, alkyl iminopropionates, alkyl iminodipropionates, alkyl amphopropylsulphonates, alkylbetaines, alkylamido-propylbetaines, alkylsultaines and alkylamidopropyl-hydroxysultaines. In this list, alkyl is understood in the sense of C10 to C14 hydrocarbon-based chains and more especially lauric, coconut or palm kernel fatty acid residues or equivalent sources. Cocoamidopropylbetaines are amphoteric compounds that are preferred for preparing the formulations according to the invention.
Undecylenamidopropylbetaine, which is the characteristic amphoteric compound of the invention, is an undecylenic-based alkylamidopropylbetaine. It can be prepared according to processes known to those skilled in the art, in particular by following the procedure described in US patent 3,225,074 (American Cyanamid) which consists in reacting undecylenic acid with N,N-dimethyl-l,3-propanediamine (DMAPA) between 140 and 200°C, followed by reacting the tertiary amidoamine
(Formula Removed)
thus obtained with monochloroacetic acid in the presence of an alkaline salt or the corresponding salt of this acid, the reaction being carried out in aqueous medium. The alkali metal chloride, usually sodium
chloride, co-produced during the reaction is generally left in this aqueous betaine solution.
The compositions of the invention are aqueous solutions in which the content of all of the constituents of the washing base (amphoteric and anionic compounds) lies within certain limits so as to ensure their physical equilibrium, in particular their homogeneity and their transparency (in the absence of the intentional introduction of pearlescent agents), these limits naturally being capable of varying to a certain extent depending on the individual components used, which will be represented by the following symbols: An used for anionic components, Amph for amphoteric compounds, ΣAmph representing all of the amphoteric compounds, AmphU representing undecylenic betaine, Amph* representing the amphoteric components except for undecylenic betaine.
This gives, on the one hand, as regards the anionic components/amphoteric compounds equilibrium:
12.5% ≤ An + EAmph ≤ 17.6
5% ≤ An ≤ 15
3 .5% ≤ ΣAmph ≤ 9.2
on the other hand, as regards the amphoteric compounds/undecylenic amphoteric component equilibrium:
3.5% ≤ EAmph ≤ 9.2
2% ≤ Amph* ≤ 7
1.5%
≤ AmphU ≤ 3.5
A common shampoo composition according to the invention will have, for example, the general composition
Sodium lauryl ether sulphate 5 to 15%
Cocoamidopropylbetaine 2 to 7%
Undecylenamidopropylbetaine 1.5 to 5.0%
Ordinary ingredients of shampoo formulations and
demineralized water qs 100%
The common ingredients in the formulation of products of this type form part of these compositions, namely:
- thickeners intended to give the shampoos a sufficient consistency and improved cosmetic qualities. Ambng the known thickeners, carbomers (acrylic acid homopolymers crosslinked with an allylic ether of pentaerythritol, of sucrose or of propylene), PEG esters, laurylpyrrolidone, acrylic copolymers and cationic polymers of natural or synthetic origin, including certain polyquaternium compounds (see the conditioners below) give very satisfactory results in the application considered, in particular bearing in mind that viscosities of greater than 1000 mPa.s, preferably between 1000 mPa.s and 30,000 mPa.s, could be obtained with these specific products ("Carbopol
Ultrez® 10" from BF Goodrich, "Atlas®G-1821" from ICI,
CR) CR}
"Surfadone LP 300" from ISP, "Acrysol 22" from Rohm &
(R") (R)
Haas, "Jaguar C 162" and "Rhodicare T" from Rhone-
® Poulenc, "Ucare Polymer Jr. 400" from Amerchol,
"Mackernium 7" from Jan Dekker/Maclntyre and "Gafquat 755 N11 from ISP). These specific thickeners make it possible to obtain acceptable viscosities when they are used at concentrations of between 0 and 4% by weight relative to the whole composition, preferably between 0.2 and 2% by weight.
- Conditioners, these being products intended
to improve the cosmetic properties of detergent
solution, generally cationic or amphoteric polymers,
oils, and in particular silicones or silicone
derivatives, the compatibility of which with all of the
other constituents of the formulation should be
checked, and in particular in order to avoid the
formation of cosmetically unacceptable cloudy gels; in
this respect, it has been found that the use of
cationic polymers such as polyquaternium-7 (in
particular "Mackernium 7" from Jan Dekker/Maclntrye),
polyquaternium-10 (in particular "Ucare Polymer JR 400"
from Amerchol) and polyquaternium-11 (in particular
"Gafquat 755 N" from ISP) at concentrations of about 1
to 4%, allow entirely clear gels to be conserved.
- Foam enhancers/stabilizers, these being
compounds taken from the group consisting of
diethanolamine alkanolamide or tertiary amine oxides,
which can be used at contents of between 1 and 5% by
weight relative to the total weight of the composition,
but which are increasingly tending to be left out of
the formulation for fear of the toxicity induced by some of their possible impurities.
The compositions can also contain certain adjuvants that are common in the shampoo sector, preserving agents, sequestering agents, softeners, foam modifiers, dyes, pearlescent agents, moisturizers, antiseborrhoeic agents, vitamins, sunscreens and fragrances. As regards the fragrances in the formulation, it should be pointed out that the low characteristic odour of undecenylamidopropylbetaine permits any fragrance, from the most discreet to the most specific.
The use, alone or as a mixture, of common preserving agents such as phenoxyethanol, methylparaben, ethylparaben, propylparaben and butylparaben (CTFA nomenclatures, INCI, 6th edition) at concentrations of between 0.25% and 1% by weight relative to the whole composition, has proven to be particularly useful for obtaining effective and long-lasting protection of foaming gels.
The compositions according to the invention can also contain additional solvents, for example glycols or glycerol, which, at concentrations of between 2% and 8% by weight, and even more particularly between 4% and 6% by weight, relative to the whole Composition, improve the physical stability of the formulations at low temperatures (problems of clouding or of crystal growth in particular) and promote rapid
penetration of the active principle into the horny layer and improve the condition of irritated horny layer (hydration of the surface epidermal layers of the scalp).
The pH of these compositions must be between 4.5 and 7.0, especially around 6, in order for the antifungal activity to be preserved at the optimum level. Adjustment of the pH to the desired value is conventionally carried out by addition of an organic or inorganic acid or base, for example citric acid, succinic acid, phosphoric acid, sodium hydroxide or sodium carbonate.
The washing and antifungal compositions according to the invention are stable (absence of decantation or of demixing of phases) and homogeneous over time within a temperature range between 4 and 45°C, both in natural light and under our Sun Test ageing conditions. They are well tolerated by the skin. They also have good foaming and washing power, which allows the removal of dandruff and good rinsability. Their viscosity must be sufficient for them to be easy to measure out in the hand. In practice, their viscosity must be greater than 1000 mPa.s.
The formulations according to the invention can be used for the preparation of more or less viscous, very faintly coloured transparent products of liquid or gel texture.
The gel forms are preferred for the curative, topical-route treatment of dandruff, these forms being used as shampoos, i.e. they are applied to the skin, the hair and/or the scalp for a few minutes, and then rinsed with water.
Concrete examples of formulations will illustrate the invention.
According to the present invention there is provided aqueous shampoo compositions containing a washing base consisting of an anioninc surfactant and an amphoteric surfactant, in which the anioninc surfactant is taken, alone or as a mixture, from the group consisting of (C1Q to C14) alkyl sulphates and (C10 to C14) alkyl ether sulphates and the amphoteric surfactant is taken, alone or as a mixture, from the group consisting of alkyl amphocarboxyglycinates, alkyl amphocarboxypropionates, alkyl amphodiacetates, alkyl amphodipropionates, alkyl amphoglycinates, alkyl amphopropionates, alkyl iminopropionates, alkyl iminodipropionates, alkyl amphopropyl sulphonates, alkylbetaines, alkylamido-propylbetaines, alkylsultaines and alkylamidopropyl-hydroxysultaines, wherein
some of the amphoteric surfactant is an undecylenamidopropylbetaine.
EXAMPLES
The compositions described below are
expressed as weight percentages.of active materials. The weight percentages of the crude products or of the corresponding commercial products used have been specified.
The undecylenamidopropylbetaine used in these examples was synthesized according to the procedure described above. Its composition is established as follows:
Undecylenamidopropylbetaine 30.0 ± 2%
NaCl 6% max.
Undecylenic acid 0.5% max.
Amidoamine 0.5% max.
Sodium monochloroacetate Its pH at 5% in water is from 5.8 to 7.5 and its Hazen colour is less than 300.
Example 1: Compared efficacy of undecylenamidopropyl-betaine and Octopyrox.
The antidaridruff and seboregulatory efficacy tests were carried out over a period of 15 days, on a
Test Panel of 20 individuals whose demographic characteristics are as follows:

(Table Removed)
a) Antidandruff action
® Undecylenamidopropylbetaine (Amphoram® U from CECA S.A.)
was compared with piroctone olamine (CFTA) or l-hydroxy-4-methyl-6-(2,4,4-trimethylpentyl)-
2(1H)pyridone; ethanol (1:1) salt (RN=68890-66-4),
® taken in its commercial form as Octopyrox (Hoechst),
at the minimum inhibitory doses (M.I.C.) for Pityrosporum ovalae, i.e., respectively, 2% and 0.2% beforehand. The results of this comparative study, expressed as a percentage of variations on D15 relative to Dl, are presented in the following table:

(Table Removed)
b) Sebumetry results
The results of the sebumetry index, measured with the
sebumeter sold by the company Courage-Khazka, expressed
as a percentage of variation on D15 relative to Dl, are presented in the following table:

(Table Removed)
From this set of results, it is concluded:
- that the state of dandruff of the 20 individuals was
improved (about 30 to 40% decrease in the area occupied
and increase in the dandruff removal index) with
Amphoram U whereas it remained stable with Octopyrox;
- that the sebumetry level did not vary significantly,
irrespective of the product used, which demonstrates
the absence of irritation.
No side effects were recorded, irrespective of the product used.
Example 2: Transparent, viscous antidandruff shampoo
Sodium lauryl ether sulphate (1) 8.4
Cocoamidopropylbetaine (2) 3.0
Undecylenamidopropylbetaine (3) 2.0
(4)
Diethanolamine laurylamide 2.0
Preserving agent, fragrance qs
Citric acid qs
Demineralized water qs 100
Commercial products used
(1) Ewpicol ® ESB 3M (Albright & Wilson) for
28%
(R)
(2) AmphoramC® 30 (CECA) for 10%

(3) Amphoram®U (CECA) 6.6%
(R)
(4) Mackamide® LMD (Maclntyre) for 2%
Characteristics
• Viscous shampoo (viscosity, measured with a
Brookfield R5 V10 viscometer, of 12,800 mPa.s), flows
well from a bottle, spreads well on the hair, totally
transparent and colourless (colour = 40 Hazen), pH =
6.6.
• Stable formulation, tested at +4°C and +45°C
(exposure for 1 month to natural light behind glass,
310 nm) and Suntest (15 days of accelerated ageing in
Suntest-type apparatus, power 500 watt/m , 300 to
800 nm);
• Forms an excellent, stable, copious white foam which
is easy to rinse out.
Example 3: Transparent and very viscous antidandruff shampoo for stubborn dandruff
Sodium lauryl ether sulphate 1 8.4
Cocoamidopropylbetaine (2) 4.5
Undecylenamidopropylbetaine (3) 3.0
Diethanolamine laurylamide (4) 2.0
Preserving agent, fragrance qs
Citric acid qs
Demineralized water qs 100
Commercial products used
(1) Empicol®ESB 3M (Albright & Wilson) for
28%
(B(2) Amphoram ®C 30 (CECA) for 15%
(R)
(3) Amphoram ® U (CECA) 9.9%
®
(4) Mackamide® LMD (Maclntyre) for 2%
Characteristics
• Very viscous shampoo (viscosity, measured with a
Brookfield R5 V10 viscometer, of 31,000 mPa.s)
• Totally transparent and colourless (colour:
60 Hazen).
• pH : 6.1.
• Stable formulation, tested at +4°C and 45°C (1 month)
and Suntest (15 h).
• Forms an excellent, stable, copious white foam which
is easy to rinse out.
Example 4: Transparent, low-viscosity antidruff shampoo shampoo
Sodium lauryl ether sulphate (1) 7.5
Cocoamidopropylbetaine (2) 3.0
Undecylenamidopropylbetaine (3) 2.0
Preserving agent, fragrance qs
Sodium chloride 1.0
Demineralized water qs 100
Commercial products used
®
(1) Empicol ESB 3M (Albright & Wilson) for
25%
(S)
(2) Amphoram® C 30 (CECA) for 6.6%
(3) Amphoram®U (CECA) 9.9%
Characteristics
• Totally transparent and colourless fluid shampoo
• Flows well from a bottle, spreads well on the hair
• Excellent, stable, copious white foam, which is easy
to rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.2
• Viscosity (Brookfield R5 V100): 1040 mPa.s
• Colour: 129 Hazen
Example 5: Transparent, viscous antidandruff shampoo
Sodium lauryl ether sulphate (1) 8.4
Cocoamidopropylbetaine (2) 4.5
Undecylenamidopropylbetaine (3) 2.0
Sodium chloride 0.5
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(1) Empicol® ESB 3M (Albright & Wilson) for
28%
(B)
(2) Amphoram® C 30 (CECA) for 151-
(3(3) Amphoram® U (CECA) 6.6%
Characteristics
• Totally transparent and colourless viscous shampoo
• Flows well from a bottle, spreads well on the hair
• Excellent, stable, copious white foam, which is easy
x> rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.2
• Viscosity (Brookfield R5 V10): 10,600 mPa.s
• Colour: 88 Hazen
Example 6: Transparent, low-viscosity antidandruff
shampoo
Sodium lauryl ether sulphate 1 6.3
Cocoamidopropylbetaine (2) 6.3
Undecylenamidopropylbetaine (3) 2.0
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(R)
(1) Empicol ESB 3M (Albright & Wilson) for
25%

(2) Amphoram® C 30 (CECA) for 15%

(3) Amphoram ®U (CECA) 6.6%
Characteristics
• Transparent and colourless fluid shampoo
• Flows well from the bottle, spreads well on the hair
• Excellent, stable, copious white foam, which is easy
to rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.0
„• Viscosity (Brookfield R5 V100) : 2300 mPa.s
• Colour: 50 Hazen
Example 7: Opaque, gelled, viscous antidandruff shampoo
Sodium lauryl ether sulphate (1) 7.5
Cocoamldopropylbetaine (2) 4.5
Undecylenamidopropylbetaine (3) 2.0
Carbomer (5) 0.9
99% triethanolamine 1.0
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(1) Empicol®ESB 3M (Albright & Wilson) for
25%

(2) Amphoram® C 30 (CECA) for 15%
(3) Amphoram®U (CECA) 6.6%
(S) (5) Carbopol Ultrez 1.0%
Characteristics
• Opaque viscous shampoo
• Flows well from the bottle, spreads well on the hair
• Excellent, stable, copious white foam, which is easy
to rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 5.1
• Viscosity (Brookfield R5 V10): 10,500 mPa.s
Example 8: Pearlescent, white, silky antidandruff
shampoo
Sodium lauryl ether sulphate (1) 7.5
Cocoamidopropylbetaine (2) 4.5
Undecylenamidopropylbetaine (3) 2.0
Carbomer (5) 0.9
Glycol stearate (6) 2.0
99% triethanolamine 1.0
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(8)
(1) Empicol ESB 3M (Albright & Wilson) for
25%
(2) Amphoram®C 30 (CECA) for 15%

(3) Awphoram® U (CECA) 6.6%
(5) Carbopol Ultrez® 1.0%
(R)
(6) Cutina ® AGS, 2.0%
Characteristics
• Pearlescent white shampoo, beautiful, rich, milky and
viscous appearance
• Flows well from the bottle, spreads well on the hair
• Excellent, dense white foam, which is easy to rinse
out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 5.1
• Viscosity (Brookfield R5 V10): 20,000 mPa.s
Example 9: Fluid, transparent, gelled antidandruff
shampoo
Sodium lauryl ether sulphate ll) 7.5
Cocoamidopropylbetaine (2) 3.0
Undecylenamidopropylbetaine (3) 2.0
Copolymer of acrylic acid and
of C20 fatty alkyl acrylate (7) 0.6
Sodium hydroxide 0.1
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
®
(1) Empicol® ESB 3M (Albright & Wilson) for
25%
(R)
(2) Amphoram ® C 30 (CECA) for 10%
(3) Amphoram®U (CECA) 6.6%
(R)
(7) Acrysol® 22 for 2.0% Characteristics:
• Translucent fluid shampoo
• Flows well from the bottle, spreads well on the hair
• Excellent, stable, copious white foam, easy to rinse
out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.5
• Viscosity (Brookfield R5 V50): 3700 mPa.s
• Colour: 204 Hazen
Example 10: Transparent, low-viscosity antidandruff
shampoo
Sodium lauryl ether sulphate (1) 7.5
(2)
Cocoamidopropylbetaine 3.0
Undecylenamidopropylbetaine (3) 2.0
(8)
Polyquaternium-10 2.0
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used

(1) Empicol ® ESB 3M (Albright & Wilson) for
25%

(2) Amphoram® C 30 (CECA) for 10%
(3) Amphoram®U (CECA) 6.6%
(8) Ucare Polymer JR 400 for 2.0%
Characteristics:
• Translucent fluid shampoo
• Flows well from the bottle, spreads well on the hair
• Excellent, stable, copious white foam, easy to rinse
out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.2
• Viscosity (Brookfield R5 V100): 1880 mPa.s
• Colour: 78 Hazen
Example 11: Transparent, low-viscosity, gentle antidandruff shampoo (8/2 = HB 1.122 A)
Sodium lauryl ether sulphate (1) 12 . 0
Cocoamidopropylbetaine (2) 3.6
Undecylenamidopropylbetaine 3 2.0
(9)
Polyquaternium-7 0.3-0.4
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(1) Empicol®ESB 3M (Albright & Wilson) for
40%
(2) Amphoram®C 30 (CECA) for 12%(3) Amphoram ® U (CECA) 6.6% (S)
(9) Mackernium ® 7 for 4.0% Characteristics :
• Transparent, colourless fluid shampoo
• Flows well from the bottle, spreads well on the hair
• Excellent soft foam, easy to rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.7
• Viscosity (Brookfield R5 V100): 1400 mPa.s
• Colour: 44 Hazen
Example 12: Very gentle pearlescent white antidandruff
shampoo for frequent use
Sodium lauryl ether sulphate (1) 9.0
(2)
Cocoamidopropylbetaine 2.4
Undecylenamidopropylbetaine (3) 2.0
Sodium methylcocoyl taurate (10) 3.0
Glycol distearate (6) 2.0
Polyquaternium-11 (11) 0.4
Laurylpyrrolidone (12) 2.0
Preserving agent, fragrance qs
Demineralized water qs 100
Commercial products used
(1) Empicol®ESB 3M (Albright & Wilson) for
30%
(2) Amphoram®C 30 (CECA) for 8.0%
(R)
(3) Amphoram ® U (CECA) 6.6%
® (9) Mackernium ® 7 for 4.0%

(10) Cutina ® ACS 2.0%
(S)
(11) Gafquat ® 755 N for 2.0%
(12) Surfadone ® LP 300 for 2.0%
Characteristics :

• Pearlescent white viscous shampoo
• Pours well from the bottle, spreads well on the hair
• Excellent white foam, easy to rinse out
• Stable formulation, tested at +4°C and +45°C (1 month
in natural light) and Suntest (15 h 00 in the Suntest)
• pH : 6.6
• Viscosity (Brookfield R5 V10) : 18,300 mPa.s
The present Composition is a syneigestic Composition when the ingradiants are
not hating chemically that ingracting synrgistally to render unepeded properties the exposition os not a meread mistare.




CLAIM;-
1. A process for preparation of aqueous antifungal and anti dandruff shampoo composition comprising a washing base consisting of an anionic surfactant and an amphoteric surfactant, in which the anionic surfactant is taken, alone or as a mixture, from the group consisting of (C1Q to C14) alkyl sulphates and (C10 to C14) alkyl ether sulphates and the amphoteric surfactant is taken, alone or as a mixture, from the group consisting of alkyl amphocarboxyglycinates, alkyl amphocarboxypropionates, alkyl amphodiacetates, alkyl amphodipropionates, alkyl amphoglycinates, alkyl amphopropionates, alkyl iminopropionates, alkyl iminodipropionates, alkyl amphopropyl sulphonates, alkylbetaines, alkylamido-propylbetaines, alkylsultaines and alkylamidopropyl-hydroxysultaines, wherein
some of the amphoteric surfactant is an undecylenamidopropylbetaine, distributing the anionic and amphoteric components, on the one hand, for the anionic components/amphoteric compounds equilibrium, as per the range of weight relative to said composition given below: 'An + Amph' lies within the range of 12.5% to 17.6% 'An' lies within the range of 5% to 15% ' Amph' lies within the range of 3.5% to 9.2%.
on the other hand, as regards the amphoteric compounds/undecylenic amphoteric component equilibrium, the ranges are:
' Amph' lies within the range of 3.5% to 9.2% 'Amph*' lies within the range of 2% to 7% 'AmphU' lies within the range of 1.5% to 3.5% in which

'An' is used for anionic components, 'Amph' for amphoteric
compounds,
' Amph' represents all of the amphoteric compounds,
'AmphU' represents undecylenamidopropylbetaine,
'Amph*' represents the amphoteric compounds except for
undecylenamidopropylbetaine.
2. The process as claimed in claim 1, wherein the anionic
surfactant is a lauryl ether sulphate and the amphoteric
surfactant is a cocoamidopropylbetaine.
3. The process as claimed in claim 1, wherein the process
comprises the steps of mixing the following ingredients to obtain
said shampoo:
Sodium lauryl ether sulphate 5 to 15%
Cocoamidopropylbetaine 2 to 7%
Undecylenamidopropylbetaine 1.5 to 5.0%
Ordinary ingredients of shampoo formulations and demineralized
water qs 100
(per cent by weight relative to the composition).
4. A process for preparation of aqueous antifungal and anti
dandruff shampoo composition, substantially as hereinbefore
described with reference to the foregoing examples.

Documents:

180-del-1999-abstract.pdf

180-del-1999-claims.pdf

180-del-1999-correspondence-other.pdf

180-del-1999-correspondence-po.pdf

180-del-1999-description (complete).pdf

180-del-1999-form-1.pdf

180-DEL-1999-Form-19.pdf

180-del-1999-form-2.pdf

180-del-1999-form-3.pdf

180-del-1999-form-4.pdf

180-del-1999-form-6.pdf

180-del-1999-gpa.pdf

180-del-1999-petition-138.pdf


Patent Number 216395
Indian Patent Application Number 180/DEL/1999
PG Journal Number 13/2008
Publication Date 28-Mar-2008
Grant Date 12-Mar-2008
Date of Filing 29-Jan-1999
Name of Patentee CESA S.A.
Applicant Address 4/8 COURS MICHELET, 92800, PUTEAUX - (HAUTS-DE-SEINE), FRANCE
Inventors:
# Inventor's Name Inventor's Address
1 REGINE DE MESANSTOURNE 42, RUE DE LA MUETTE, 78600 MAISONS-LAFITTE, FRANCE
2 HELENE LEBON 29 ROUTE DE VERSAILLES,78430 LOUVECIENNES, FRANCE
3 HELENE LE GALL 2, ALLEE DE SULLY, 91170 VIRY CHATILLON, FRANCE
PCT International Classification Number A61K 7/75
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 98.01771 1998-02-13 France