COMPLETE AFTER PROVISIONAL LEFT ON 9/10/06
FORM 2
THE PATENTS ACT. 1970
(39 OF 1970)
&
THE PATENT RULES, 2003
COMPLETE SPECIFICATION [SECTION 10; RULE 13]
"A COMPOSITION FOR COLOURING KERATIN FIBERS AND A METHOD OF PREPARATION THEREOF"
GODREJ CONSUMER PRODUCTS LIMITED, AN INDIAN COMPANY INCORPORATED UNDER THE COMPANIES ACT, 1956, HAVING ITS REGISTERED OFFICE AT PIROJSHANAGAR, EASTERN EXPRESS HIGHWAY, VTKROLI, MUMBAI - 400079, MAHARASHTRA STATE, INDIA.
THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE NATURE OF THIS INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED: -


9 OCT 2006

FIELD OF INVENTION:
The present invention relates to a composition for colouring keratin fibers such as hair and a method of preparation thereof. The said composition is made from products of natural origin.
BACKGROUND OF THE INVENTION:
The most prevalent early practice of colouring keratin fibers such as hair (hereinafter referred to as keratin fibers or hair) is the use of natural colour from the leaves of Henna (Lawsonia inermis) plant. Another plant, Indigo (Indigofera tinctoria) has also been used, primarily/for dyeing keratin fibers. Both Henna and Indigo have limited variations in imparting colour to keratin fibers. The former imparts red-orange hue to the keratin fibers, while the latter gives blue to violet colour, that too only on grey keratin fibers. Often these colours are not the choice of the consumers as they do not go well with the black keratin fibers. These factors undermine and limit their use primarily for hair colourants in comparision to synthetic hair colours, which provide wide variation of colours and effective hair colouration. However synthetic colours are associated with certain drawbacks, namely allergies in humans. Increasingly, consumers are looking for natural products or product formulations based on these are considered to be safe and milder than the synthetic products.
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PRIOR ART:
There are several patents using synthetic dyes, precursors to dyes, coupling agents, oxidizing agents etc. Alternate to synthetic dyes have also been developed, from time to time, using plant extracts/parts. Henna and indigo have also been used as hair colours with some specific plant extracts and synthetic dyes/enzymes etc.
US Patent 4,183,366 describes henna-based hair coloring and/or hair conditioning compositions comprising of henna powder, a non-ionic surface active agent, a water soluble polymer and a quaternary salt.
US Patent 5,042,989 describe a process of dyestuffs from parts of plants. The plant materials suggested in this patent dyer's furze, dyer's woad, dyer's esade, indigo and redwood.
US 6,139,853, 853 describes a hair colorant with 25 to 70% of henna (similar range as the current invention) but has oxidizing agent added to the colorant.
US Patents 6,656,229 & 6,849,096 describe a hair dye formulation primarily composed of a dye component including indicant derived from indigo plants and a formulation primarily composed of a beta-glucosidase enzyme component. Hair is first mordanted with such as aluminium, iron and the like.
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Although heena and indigo are known colouring agents, a mere combination of the aforesaid two ingredients fail to give a natural colouration, thereby not giving the desired result, both in terms of colour development and its substantively. Moreover, there is an inherent tendency of the mixture of heena and indigo to first impart a green colour on the hair, which gradually changes to various other shades over a period of time, which aesthetically and from the point of cosmetics is not the colour of choice for the consumers.
OBJECT OF THE PRESENT INVENTION:
The present invention obviates the aforesaid drawbacks by providing a composition and a process of preparation thereof, resulting into a definite hair colouration of a brownish-black shade, most accepted and akin to human hair.
SUMMARY OF THE PRESENT INVENTION:
The present invention proposes a composition for colouring keratin fibers comprising of (i) 40 to 85 % w/w indigo powder, (ii) 15 to 60 % w/w Henna powder, (iii) 0.5 to 5 % w/w cellulose gums described herein, (iv) 0.5 to 5% w/w saponin, (v) 0.5 to 5 % w/w nutrient like Amla (Emblica Officinalis) and/or Bhringaraj (Eclipta Prostrata / Alba) and/or Brahmia (Centellaa Asiatica) and/or Jaswant (Hibiscus Rosasinensis) and (vi) 0.5 to 4 % w/w Citric acid.
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It further proposes a method of preparing indigo powder comprising of sun-drying indigo leaves cut from 90 days to 110 days old indigo plants; pulverizing the said sun-dried leaves; putting the pulverized leaves through sieve to obtain powder having particle size 80 microns to 200 microns. Still further it proposes a composition using indigo powder prepared by said method.
It also proposes a method of preparing the said composition in which 40 to 85 % w/w indigo powder prepared by the said method is mixed with 15 to 60 % w/w of Heena powder of particle size 80 microns to 200 microns and cellulose gums of 0.5 to 5 % w/w are then added into the said mixture together with 0.5 to 5 % w/w of the said nutrients and 0.5 to 4 % w/w of citric acid and the whole mass is pulverized for 45 minutes to 70 minutes.
DETAILED DESCRIPTION OF THE PRESENT INVENTION:
INDIGO HAR VESTING
The maturity of indigo leaves at which they are to be harvested during the life
cycle of the indigo plant and their consequent method of drying, plays a very
critical role in the composition according to this invention, to obtain the desired
colouration.
The US Patent # 6,849,096 speaks only about harvesting fresh indigo leaves collected from the top portion of the growing indigo plants and their consequent drying. The patent fails to elaborate the life cycle stage of the indigo plant at which the leaves are to be harvested.
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It has been the inventor's observation, (critical to the development of the final colouration) based on several experiments with the indigo leaves harvested at different time periods of Indigo plant's life cycle that the desired colouration from the leaves was obtained only when the leaves were harvested after the indigo plants started to flower, preferably after ninety days of cultivation and most preferably between 100 days to 110 days of cultivation.
SUN-DRYING
Consequent to harvesting of the indigo leaves at the most appropriate time, as described above, a controlled sun-drying technique is equally critical for the harvested indigo leaves. Since changes in colouration during harvesting or immediately thereafter during the drying are of grave consequence to the composition according to this invention, it is therefore necessary to complete a particular harvesting cycle and the consequent drying process rapidly.
The indigo leaf plucked as aforesaid are pulverized and put through sieve to obtain powder having a determined granulometry, wherein the grain ranges from 80 microns to 200 microns, preferably from 120 microns to 150 microns.
Other methods of drying of indigo leaves were experimentally tried; the observations are summarized as follows:
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OVEN DRYING
Freshly harvested Indigo leaves were dried in an oven at 55°C for 2 hours, 4 hours and 6 hours. The moisture content was recorded as 62.15%, 37.07% and 8.2% respectively. Oven drying was again repeated with freshly harvested indigo leaves at 7.0°C for 2 hours and 4 hours with the moisture content being recorded as 24.24% and 4% respectively. The oven dried leaves from these experiments were powdered and used in the inventive formulation but they failed to give the desired colouration.
VACUUM DRYING
Freshly harvested indigo leaves were dried in a vacuum oven at 60°C for 1 hour and 4 hours. The drying of the leaves was not uniform with the only one side getting dried while the other side retaining moisture. Vacuum drying was found to be an inappropriate method for drying indigo leaves for the said inventive formulation.
MICRO WA VE DRYING
Freshly harvested indigo leaves were micro waved for 5 minutes with 10 second bursts. The drying was not uniform. The powder so obtained was used in the inventive formulation but it failed to give the desired colouration.
Following observations were noticed when the Indigo leaves were processed by different drying methods:
1) By Sun drying method Indican content in the leaves was 20 to 24 mg per
kg-
2) By Oven drying method Indican content in the leaves was 2 to 5 mg per
kg--
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3) By Vacuum drying method Indican content in the leaves was 3 to 5 mg per kg.
4) By micro-oven drying method Indican content in the leaves was 5 to 6 mg per kg.
According to this invention, a preferable composition should contain minimum 16 mg per kg of Indican in the Indigo leaves, then only the brown-black colour will form on keratin fiber.
Indican (Indoxyl-(b-D-glucoside) is a precursor of the Blue dyes Indigo and is present in large amount in Indigo leaves. When leaves are broken then indicant is hydrolyzed to indoxyl and glucose by the native enzymes like (3-glucosidase. Indoxyl is finally converted into Blue indigo by air oxidation. When indigo plants are 100 days old, Indican content in the leaves is about 24 to 28 mg per kg on dry basis.
The Henna powder used in the composition of this invention should be colour imparting henna powder. The minimum lawsone content in the henna should be more than 1 percent. The Henna powder should be dehydrated, pulverized and sieved to produce powder having a determined granulometry, where in the grain ranges from 80 microns to 200 microns, preferably from 120 microns to 150 micrones.
The saponin containing Aritha or Shikaki is used in the composition. Aritha helps in easy application of composition on head. The thickeners used in the
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present invention include Xanthan gums, Carboxymethyl celluloses, Gaur gums and cationic derivatives thereof. Preferably the amount of thickener to be used is from 0.5 % w/w to 4 % w/w, preferably from about 1 % w/w to 2 % w/w of Cationic derivative of Gaur gum. Nutrient mixture adjuvant like Amla (Emblica officinalis), Bhringaraj (Eclipta prostrata/alba), Brahmi {Centella asiatica) & Jaswant (Hibiscus rosasinensis) helps in colour pick up, preferably in the range of 0.5 % w/w to 2 % w/w. More than 2 % w/w interferes in colour. Normally the above composition has more than 5pH. The pH level is adjusted between 4pH and 5pH with the addition of citric acid. Optimum colour pick up takes place between 4pH and 5pH.
The present invention will now be explained with the help of the following examples and the said examples in no way limit the scope of this invention.
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EXAMPLES:
Example No.l
Composition for the grey hair is prepared having the following formulation:

Ingredients Weight percent
Indigo powder 60
Henna powder 37.1
Cationic guar gum 1
Citric acid 0.5
Aritha powder 1.0
Amla (Emblica officinalis) 0.1
Bhringaraj (Eclip ta prostrata/alba) 0.1
Brahmi (Centella asiatica) 0.1
Jaswant (Hibiscus rosasinensis) 0.1
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Example No.2
Composition for the grey hair is prepared having the following formulation:

Ingredients Weight percent
Indigo powder 65
Henna powder 31.6
Cationic guar gum 1
Citric acid 1.0 •
Aritha powder 1.0
Amla (Emblica officinalis) 0.1
Bhrigaraj(Eclipta prostrata/alba) 0.1
Brahmi {Centella asiatica) 0.1
Jaswant {Hibiscus rosasinensis) 0.1
To use the above formulations, preferably about 1 part, of one of the above compositions, are mixed with warm (60° C) water to a smooth consistency and applied to freshly shampooed hair. Keep it for 90 minutes to 120 minutes and then rinsed with plain water. Hair treated with above compositions of this invention will show lustrous, brownish black hair.
ADVANTAGES:
1) Gives a natural soft colour.
2) Provides good conditioning benefit to the human hair and the keratin fibers.
3) Provides a natural looking soft colour to grey human hair and keratin fibers.
4) Provides colouring and conditioning benefits without the use of harsh moderants in the composition.
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5) Time saving.
6) Long lasting.
7) Convenient.
WE CLAIM:
1) A composition for colouring keratin fibers comprising of (i) 40 to 85 % w/w
indigo powder, (ii) 15 to 60 % w/w Henna powder, (in) 0.5 to 5 % w/w herein
described cellulose gums, (iv) 0.5 to 5% w/w saponin, (v) 0.5 to 5 % w/w
nutrient like Am la (Emblica Officinalis) and/or Bhringaraj (Eclipta Prostrata /
Alba) and/or Brahmi (Centella Asiatica) and/or Jaswant (Hibiscus
Rosasinensis) and (vi) 0.5 to 4 % w/w Citric acid.
2) A method of preparing indigo powder comprising of sun-drying indigo leaves cut from 90 days to 110 days old indigo plants; pulverizing the said sun-dried leaves; putting the pulverized leaves through sieve to obtain powder having particle size 80 microns to 200 microns.
3) A composition as claimed in claim 1 above wherein, the indigo powder is prepared by the method described and claimed herein.
4) A method of preparing the composition as claimed in claim 1 above wherein, 40 to 85 % w/w indigo powder prepared by the method in claim 2 above is mixed with 15 to 60 % w/w Heena powder of particle size 80 microns to 200 microns, herein described cellulose gums of 0.5 to 5 % w/w are then added into the said mixture together with 0.5 to 5 % w/w herein described
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nutrients and 0.5 to 4 % w/w citric acid and the whole mass is pulverized for 45 minutes to 70 minutes.
5) A Composition as claimed in claim 1 above wherein, indigo powder is 65 to
75 % w/w, henna powder is 25 to 35 % w/w, cellulose gum is 1 to 2 % w/w,
saponin is 1 to 3 % w/w, nutrient is 0.5 to 2 % w/w and citric acid is 0.5 to 4 %
w/w.
6) A method as claimed in claim 4 above wherein, indigo powder is 65 to 75 % w/w, henna powder is 25 to 35 % w/w, cellulose gum is 1 to 2 % w/w, saponin is 1 to 3 % w/w, nutrient is 0.5 to 2 % w/w and citric acid is 0.5 to 4 % w/w.
7) A composition as claimed in claim 5 above wherein, saponin is Aritha.
8) A method as claimed in claim 6 above wherein, saponin is Aritha.
9) A composition substantially as herein described.
10) A method substantially as herein described.
Dated this 7lh day of Oct' 2006.

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ABSTRACT
The present method proposes a composition for colouring keratin fibers comprising of (i) 40 to 85 % w/w indigo powder, (ii) 15 to 60 % w/w Henna powder, (iii) 0.5 to 5 % w/w cellulose gums, (iv) 0.5 to 5% w/w saponin, (v) 0.5 to 5 % w/w nutrient like Amla (Emblica Officinalis) and/or Bhringaraj (Eclipta Prostrata / Alba) and/or Brahmi (Centella Asiatica) and/or Jaswant (Hibiscus Rosasinensis) and (vi) 0.5 to 4 % w/w Citric acid.

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9 OCT 2006