DESC:FIELD OF THE INVENTION
The present invention relates to a novel composition comprising a one or more natural ingredients as dyeing or coloring agents for personal care applications, and a method of making the same.

BACKGROUND OF THE INVENTION
Natural ingredients, particularly plant extracts have been used in personal care products since a long time. With increasing demand for natural products including food, personal care and medical products, there has been significant research on the use of extracts of plants or herbs for incorporation in such compositions. Over the years, researchers have been working on finding safe, non-toxic hair dyes such as plant extracts based formulations that can replace chemical hair dyes while also rendering better hair color effects. Research is in progress to ensure that little to no synthetic chemical is used while extracting natural products, and no chemical additive is added to the final product. Natural products while being sustainable, are also eco-friendly to our planet.
WO2010063533 A1 relates to a method of coloring keratinous fibers, especially human hair, and a kit for its implementation. The keratinous fibers are contacted sequentially with a pre-treatment composition and a color developer, wherein the pre-treatment composition comprises an iron salt including a reducing agent, a buffer, and a penetration enhancer that are mixed not more than 360 minutes prior to contacting the keratinous fibers, and the color developer is hydrolysable tannin or its breakdown products or derivatives obtained from a natural or synthetic source. The hydrolysable tannins employed are gallic acid, tannic acid, catechins, or polyphenols. The natural sources of hydrolysable tannins used in the formulation are gall nuts, Terminalia species e.g., chebula, bellerica, arjuna tea, mucuna pruriens and other gallic acid rich sources.

US 8,333,808 B2 relates to a non-oxidative permanent natural hair dyeing agent with a two-part natural hair blackening product combination, and a method of using the same. The ferrous salt acts as a mordant active and could be combined with gallic acid that naturally exists in tannins as a dye active to obtain said product. The dyeing chroma and fastness on the hair are achieved through the formation of a ferric complex in the hair.

US 8,382,856 B2 discloses a hair dye comprising a combination of substances reacting with iron to develop color and an ultraviolet absorbent having a 2-hydroxybenzophenone skeleton, and an agent containing iron salt. The substance reacting with iron to develop color is at least one type selected from tannic acid, gallic acid and a derivative thereof, gallnut, pyrogallol, logwood, hematein, catechol, salicylic acid and a derivative thereof, phthalic acid, eugenol, isoeugenol, nicotinic-acid amide, dehydroacetic acid, pyridoxine, ellagic acid, kojic acid, maltol, ferulic acid, hinokitiol, turmeric extract, curcumin, Scutellaria root extract, onion extract, quercetin, rutin, hesperetin, hesperidin, fresh coffee bean extract, caffeic acid, chlorogenic acid, tea extract, catechin, epicatechin, lithospermi radix extract, Japanese basil extract, shisonin, grape leaf extract, grape extract, enocyanin, laccaic acid, lac, cochineal, carminic acid, elderberry, red cabbage, purple sweet potato, tamarind, kaoliang, apigeninidin, and luteolinidin.

US2004241114A1 relates to an ion-pair delivery system useful for gender and ethnic selective hair and nail care applications in which an electron donor composition and an electron acceptor composition, or a proton donor composition and a proton acceptor composition, or an anionic and a cationic composition, are combined synergistically.

WO2012129961A1 relates to a hair dye composition comprising henna, medicine Terminalia fruit, pomegranate rind, and a chelator which is a water soluble salt containing an iron ion. The composition and hair dye prepared therefrom can be used to dye hair from white to brown color.

CN114699350A deals with a pomegranate peel extract based hair dye formulation. Said formulation comprises pomegranate peel extract, tannin, FeCl3.6H2O, sodium hyaluronate, aloe polysaccharide, tea saponin, NaOH, and water.

IN201711014584A is related to a natural hair dye composition comprising of different parts of herbs and medicinal plants along with grandis gum as a fixating agent. The herbs are selected from fruits of Phyllanthus emblica (Amla), seeds of Macrotyloma uniflorum Linn (Fabaceae), pods of Acacia Concinna, Curcuma longa rhizome, lemon, flowers of Punica granantum (pomegranate), Clitoria ternatea, and tea/coffee extract. The resulting dye is black or red in color depending on the herb or medicinal plant used in the formulation.

CN106137838A deals with a paste-like natural hair dye mainly comprising Indigofera tinctoria, Lawsonia inermis, Bacopa monnieri, Radix rubiae, Acacia farnesiana, Fructus phyllanthi, catechu, Coffea arabica, Herba ecliptae, a penetrant, an absorbent and a thickener.

EP3669862A2 deals with a herb based hair dye formulation comprising coloring agents, enhancing agents, a toning agent of herbal origin, and optionally auxiliary agents also of herbal origin, and a method of producing the herb based hair dye formulation. The herb based agents are herbal actives obtained by processing plant parts. Said coloring agent is Henna, Indigo, Manjistha, Turmeric, Hibiscus, Indigo extract, or any combination thereof, said enhancing agent is Amla, Brahmi, Bhringraj, Methi, or any combination thereof, said toning agent is Cassia, and said optional auxiliary agent is Reetha, Shikakai, or a combination thereof.

KR20150107427 deals with an eco-friendly dye comprising green tea extract, thioglycolic acid, magnesium carbonate, castor oil, and folic acid.

Oxidative hair dye damages hair, and may cause contact dermatitis or latent influence on the body for a long time. They could also be mutagenic or carcinogenic. Use of oxidants in hair dyes may cause skin rashes, allergies, and various other side effects. Non-oxidative hair dye products require long dyeing times, and the hair dyeing property and color tone may not be satisfactory. Ionic hair dyes are semi-permanent hair dyes, and do not damage hair. However, the ionic hair dyes are problematic in terms of skin coloration upon dyeing, and are not long-lasting.

Though several researchers have developed natural ingredients based dyeing and coloring compositions, due to poor stability, these natural ingredients based dyeing and coloring compositions must be used up once they are unsealed, which results in the wastage of resources and causes economic burden to the consumers.

Thus, there is a need to develop a personal care composition or a hair dyeing product that is safe, non-toxic, non-allergic, stable, simple, and easy to use while also minimizing wastage of material.

The present invention overcomes the aforementioned problems through the use of formulations comprising nanoparticles or microparticles of natural ingredients sourced from plant extracts.

OBJECT OF THE INVENTION
The principal object of the present invention is to provide personal care compositions comprising natural coloring agents.
Another object of the present invention is to provide hair dye compositions comprising natural coloring agents.

Yet another object of the present invention is to provide colorant compositions comprising natural coloring agents and natural dyeing agents with moisturizing capability.

Still yet another object of the present invention is to formulate personal care compositions comprising natural ingredients in solution, gel, oil, cream, paste, emulsion, or spray forms.

Yet another object of the present invention is to formulate personal care compositions in the form of a solution, suspension, emulsion, or a matrix structure.

Further another object of the present invention is to provide natural ingredients based colorant compositions that can generate different shades of colors.

Another object of the present invention is to formulate personal care compositions comprising natural ingredients which are in the form of nanoparticles or microparticles.

Yet another object of the present invention is to formulate personal care colorant compositions that are devoid of harsh chemicals such as bleaching agents, amines, ammonia, peroxide, and sulfur compounds.
Still yet another object of the present invention is to provide personal care colorant compositions that do not possess an alkaline pH.

Further yet another object of the present invention is to provide personal care colorant compositions that are devoid of surfactants, penetration agents, and viscosity enhancers.

SUMMARY OF THE INVENTION
The present invention provides novel ammonia-free, amine-free, and peroxide-free personal care compositions comprising of one or more natural ingredients for dyeing or coloring. The present invention is particularly related to compositions comprising one or more plant extracts that can generate different shades of colors depending on the quantity and ratios of the polyphenols containing plant extracts used and the duration of application of said composition. Said plant extracts may be selected from Punica granatum peel extract (pomegranate peel extract), Emblica officinalis (amla extract), and leaves of Camellia sinensis (green tea extract), Lawsonia inermis, Indigofera tinctoria, Terminalia arjuna, Tanacetum parthenium, Pterocarpus marsupium, Terminalia bellirica, Terminalia chebula, Aesculus hippocastanum, Achillea millefolium, Avena sativa, Morus alba, other polyphenol-rich sources, and combinations thereof.

The invention also relates to a method of dyeing keratin fibers comprising the application of a composition of the plant extract based formulation(s).

BRIEF DESCRIPTION OF THE DRAWINGS
The summary of the present invention, as well as the detailed description, are better understood when read in conjunction with the accompanying figures that illustrate one or more possible embodiments of the present invention, of which:
Fig. 1 represents a microscopic image of an ammonia-free, amine-free, and peroxide-free personal care composition (hair dyeing composition) comprising microparticles of natural plant extracts;
Fig. 2a represents untreated hair swatch;
Fig. 2b represents hair swatch after application of a natural ingredients based hair dye composition disclosed in example 9 for 15 days;
Fig. 2c represents hair swatch after application of a natural ingredients based hair dye composition disclosed in example 10 for 15 days;
Fig. 3 represents a shampoo comprising natural extracts as coloring agents; and
Fig. 4 represents a process flowchart for the extraction of plant extracts.

DETAILED DESCRIPTION OF THE INVENTION
The term “natural ingredients” has been used interchangeably with “plant extracts”. Also, the terms “formulations” and “compositions” have been interchangeably used. Also, the term “hair dying” and “hair coloring” have been interchangeably used. Also, the terms “coloring” and “colorant” have been interchangeably used. The term “personal care” can be interpreted as hair, moustache, beard, and nail care.

The present invention is related to ammonia-free, amine-free, and peroxide-free personal care compositions comprising one or more natural ingredients as coloring agents in specific ratios. The personal care compositions of the present invention also comprise inorganic salts, stabilizer, water, and optionally softener, excipients, carriers, or combinations thereof. Said natural ingredients comprise one or more polyphenols as active agents extracted from natural sources. The natural ingredients used in the compositions of the present invention are obtained from plant sources. The natural ingredients used in the compositions are in the form of microparticles as shown in Fig. 1.

The natural ingredients used in the preparation of said compositions in accordance with the various embodiments of the present invention may be selected from polyphenols containing plant sources. Said active agents include one or more polyphenols extracted from natural sources of tannic acid, gallic acid, ellagic acid, chebulinic acid, punicalagin, epicatechin, catechin, epigallocatechin gallate, epicatechin gallate etc. Said one or more plant sources are selected from Punica granatum, Emblica officinalis, and Camellia sinensis, Lawsonia inermis, Indigofera tinctoria, Terminalia arjuna, Tanacetum parthenium, Pterocarpus marsupium, Terminalia bellirica, Terminalia chebula, Aesculus hippocastanum, Achillea millefolium, Avena sativa, Morus alba, and other polyphenol-rich plant sources.

According to the embodiments of the present invention, said natural ingredients based compositions may further comprise one or more inorganic salts, stabilizers, water, and optionally softeners, excipients, carriers, or combinations thereof. Said compositions can be used as coloring compositions for generating different shades of brown and black color by varying the concentration in the range of 0.1% to 30%, and combination of one or more natural ingredients.

Inorganic salts used in the preparation of the coloring compositions may be an iron salt selected from ferrous gluconate, ferrous sulfate, ferrous lactate, ferrous chloride, ferrous nitrate, and ferrous fumarate.

Stabilizers used in the preparation of the coloring compositions of the present invention may be selected from ascorbic acid, cysteine, and salts or derivatives thereof.

The desired coloration from the personal care compositions of the present invention can be obtained by individual plant extract or by mixing different plant extracts in various ratios to provide different shades of color, the desired coloration may vary from black to brown shades. According to the various embodiments of the present invention, said coloring or dyeing product may be in the form of any personal care product such as shampoo, soap, gel, spray, rinse-off product, oil, cream, emulsion, and leave-on product.

The natural ingredients based compositions of the present invention can be incorporated in the preparation of various personal care compositions such as hair coloring compositions, nail coloring compositions, etc. The color and the intensity or shade can be varied by changing the concentrations and combinations of said one or more natural ingredients.

The plant extracts used in the present invention are prepared by drying and pulverizing said plant sources, extracting with organic solvents, filtering, concentrating and drying the filtrate, extracting said dried filtrate with non-polar solvents, concentrating, and drying the same. The final plant extract obtained through the above process is used in the personal care compositions of the present invention.

The preparation of said compositions comprises of:
(i) addition of extracts of natural ingredients to deionised water, and stirred at room temperature for approximately 30 minutes;
(ii) addition of inorganic salt to the solution obtained in step (i); and
(iii) addition of stabilizer to the solution obtained in step (ii), and stirred for approximately 90 minutes.

Examples
Coloring compositions can be prepared in accordance with the various embodiments of the present invention. Some of the examples are presented herein.
Example 1
A hair coloring composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said hair coloring composition.
Ingredients of Composition 1 Quantity per 100 g
Punica granatum peel extract 0.5
L-ascorbic acid 0.02
Ferrous gluconate 1
Emblica officinalis 2
Camellia sinensis Extract 2
Deionised water 94.48

Example 2
A hair coloring composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said hair coloring composition.
Ingredients of Composition 2 Quantity per 100 g
Punica granatum peel extract 0.05
L-ascorbic acid 0.02
Ferrous gluconate 1
Emblica officinalis extract 1
Deionised water 97.93
Example 3
A hair coloring composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said hair coloring composition.
Ingredients of Composition 3 Quantity per 100 g
L-ascorbic acid 0.02
Ferrous gluconate 1
Camellia sinensis extract 2
Deionised water 96.98

Composition 1, Composition 2, and Composition 3 were sprayed on hair swatches and air dried for 2 hours. They were then washed thoroughly with water and allowed to dry. It was observed that a darker shade of the color was obtained upon repeating the application process for 15 days.

Example 4
A personal care composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said personal care composition.
Ingredients of Composition 4 Quantity per 100 g
Punica granatum peel extract 1
Emblica officinalis extract 1
Ferrous gluconate 3

Example 5
A personal care composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said personal care composition.
Ingredients of Composition 5 Quantity per 100 g
Emblica officinalis extract 0.2
Camellia sinensis extract 0.2
Ferrous gluconate 1

Example 6
A personal care composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said personal care composition.
Ingredients of Composition 6 Quantity per 100 g
Emblica officinalis extract 1
Ferrous gluconate 3

Example 7
A personal care composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said personal care composition. In said composition, said Camellia sinensis extract comprises 19% catechin and 33% EGCG (epigallocatechin gallate).

Ingredients of Composition 7 Quantity per 100 g
Camellia sinensis extract 1
Ferrous sulphate 3

The ingredients of said compositions were thoroughly mixed to form homogenous mixtures. Appropriate quantity of deionized water was added to make a concentration of 0.1% to 30%. The obtained solutions of Composition 4, Composition 5, Composition 6, and Composition 7 were mixed with personal care compositions for further use.

Example 8
To a shampoo composition (Composition 8) presented in below table, Composition 4, Composition 5, Composition 6, or composition 7 of the present invention were added to obtain shampoo based coloring compositions.

Ingredients of Composition 8 % w/w (in 100 g composition)
Guar hydroxypropyltrimonium chloride 0.5
Phenoxyethanol 1
Sodium lauryl ether sulphate 30
Cocamidopropyl betaine 10
Glycerin 1
Polyquaternium - 7 3
Ethylene glycol distearate 5
Fragrance 1
PEG - 40 Hydrogenated Castor Oil 1
Sodium chloride 0.2
Citric acid 10% 0.2
Deionised water 47.1

Example 9
A hair coloring composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said hair coloring composition.
Ingredients of Composition 9 Quantity per 100 g
Camellia sinensis extract 1.6
Emblica officinalis extract 2.3
Ferrous sulphate 0.6
L-ascorbic acid 0.02
Deionised water 95.48

Example 10
A hair coloring composition of the present invention is presented below along with the quantity of the ingredients used per 100 g of said hair coloring composition.
Ingredients of Composition 10 Quantity per 100 g
Camellia sinensis extract 1.6
L-ascorbic acid 0.02
Ferrous sulphate 0.6
Deionised water 97.78

Composition 9 and Composition 10 were sprayed on hair swatches, and air dried for 2 hours. They were then washed thoroughly with water and allowed to dry. It was observed that a darker shade of the color was obtained upon repeating the application process for 15 days.

According to some embodiments of the present invention, the hair coloring compositions also possess moisturizing property. Said composition comprises 0.1 - 50% weight of natural ingredients, 0.1 - 20% weight of inorganic salt, 0.01 - 5% stabilizer, upto 98% weight of deionized water, and optionally 0.001-5% weight of one or more ingredients selected from softeners, excipients, carriers, and combinations thereof.

Performance Evaluation
Hair coloring compositions prepared in accordance with the various embodiments of the present invention were tested on hair swatches by incubating the hair swatches in the hair color solution for 2 hours. The swatches were then dried using a hair dryer. Subsequently, the hair swatches were washed well with a shampoo, rinsed with water, and dried. As can be seen in Fig. 2a, 2b, and 2c, the untreated hair swatches of Fig. 2a turned black as seen in Fig. 2b upon application of Composition 9 prepared in accordance with the embodiments of the present invention for 2 hours for 15 days, and turned dark black as seen in Fig. 2c upon application of Composition 10 prepared in accordance with the embodiments of the present invention for 2 hours for 15 days.
The present invention is also related to a method of coloring wherein the method is a non-bleached method of coloring hair, wherein said compositions have a pH of 2.5 - 6, preferably 2.5 - 4, alleviating the use of ammonia, amines, peroxide, and an alkaline pH.

The novel compositions of the present invention comprising of nanoparticles or microparticles of plant based ingredient(s) may be in the form of a paste, solution, suspension, emulsion, or matrix structure. The product may be in the form of a spray, gel, soap, cream, oil, emulsion, leave-on product, shampoo, rinse-off, or any other hair care and personal care product. Said hair coloring compositions may be applied upto 15 days for obtaining a desired shade.

The composition of the present invention is an ammonia-free, amine-free, and peroxide-free personal care composition comprising of 0.1% to 50% by weight of natural ingredients, (b) 0.1% to 20% by weight of inorganic salts, (c) 0.01% to 5% by weight of a stabilizer, (d) up to 98% by weight of deionized water, and (e) optionally, 0.001% to 5% by weight of a softener, excipients, a carrier, or a combination thereof. Said natural ingredients comprise one or more polyphenols as an active agent extracted from natural sources, wherein said natural sources of polyphenols are plant extracts selected from the group consisting of Punica granatum peel, Camellia sinensis, Emblica officinalis, Lawsonia inermis, Indigofera tinctoria, Terminalia arjuna, Tanacetum parthenium, Pterocarpus marsupium, Terminalia bellirica, Terminalia chebula, Aesculus hippocastanum, Achillea millefolium, Avena sativa, Morus alba, and combinations thereof.

The personal care compositions of the present invention are safe to use as these are devoid of any bleaching agent, harsh chemicals such as ammonia, amines, peroxide, and sulfur compounds. Said compositions are also devoid of surfactants which have an adverse effect on environment due to their high toxicity and low biodegradability. Said compositions are also devoid of penetration agents, or viscosity enhancers. It is also cost-effective due to the use of natural ingredients, while enabling a broad range of colour variations ranging from brown to deep black, as per the desired result of the end user.

It is to be understood, however, that the present invention would not be limited by any means to the components, arrangements and materials that are not specifically described, and any change to the materials, variations, and modifications can be made without departing from the spirit and scope described in the present invention.
,CLAIMS:I/We claim:
1. An ammonia-free, amine-free, and peroxide-free personal care composition comprising:
(a) 0.1% to 50% by weight of natural ingredients,
(b) 0.1% to 20% by weight of inorganic salts,
(c) 0.01% to 5% by weight of a stabilizer,
(d) up to 98% by weight of deionized water, and
(e) optionally, 0.001% to 5% by weight of additives selected from a softener, excipients, a carrier, and a combination thereof,
wherein,
said personal care composition is a coloring composition, and
said natural ingredients are selected from tannic acid, gallic acid, ellagic acid, chebulinic acid, punicalagin, epicatechin, catechin, epigallocatechin gallate, and epicatechin gallate sourced from one or more polyphenol-based plant extracts.
2. The composition as claimed in claim 1, wherein said one or more polyphenol-based plant extracts are extracts of plants selected from Punica granatum peel, Camellia sinensis, Emblica officinalis, Lawsonia inermis, Indigofera tinctoria, Terminalia arjuna, Tanacetum parthenium, Pterocarpus marsupium, Terminalia bellirica, Terminalia chebula, Aesculus hippocastanum, Achillea millefolium, Avena sativa, Morus alba, and combinations thereof.
3. The composition as claimed in claim 1, wherein the inorganic salt is an iron salt selected from ferrous gluconate, ferrous sulfate, ferrous lactate, ferrous chloride, ferrous nitrate, and ferrous fumarate.
4. The composition as claimed in claim 1, wherein the stabilizer is selected from ascorbic acid, cysteine, and salts or derivatives thereof.
5. The composition as claimed in claim 1, wherein the concentration of said natural ingredients in the composition is in the range of 0.1% to 30%.
6. The composition as claimed in claim 1, wherein said composition has a pH in the range of 2.5 to 6.
7. The composition as claimed in claim 1, wherein the composition comprises nanoparticles or microparticles formulated in the form of a paste, solution, suspension, emulsion, or any matrix structure.
8. The composition as claimed in claim 1, wherein the composition is suitable for use as a spray, gel, soap, cream, oil, emulsion, leave-on product, shampoo, or rinse-off product.