Title of Invention

A PROCESS FOR THE EXTRACTION OF ORGANIC COLOURANTS FROM PLANTS

Abstract

The present invention relates to a process for the extraction of organic colourants from plant materials. The invention also relates to process for preparation of safe, eco-friendly, health protective and beautifying herbal colors and aroma useful for cosmaceutical applications. More particularly, the invention relates to use of herbal colors in cosmaceutical applications like lipsticks, eye shadow, glow-glitters and rouges. The said colors are absolutely lipophilic in nature. The compositions prepared therefrom promote the stimulation of creative thoughts, enhance sensual feeling, induce positive mental health and help in overcoming depression.

Full Text

The present invention relates to a process for the extraction of organic colourants from plant materials. This invention particularly relates to the process of preparation of safe, eco-friendly, health protective and beautifying herbal colours and aroma useful for cosmaceutical applications. More particularly the invention relates to use of natural colours and aroma in cosmaceutical applications like functional lipstick and other cosmaceutical products like eye shadows, glow-glitters and rouges. Further, more particularly the invention relates to process of extracting safe, eco-friendly, health protective and beautifying herbal colours There is worldwide revival of interest for using herbal colours especially in cosmetics and Pharmaceuticals as the synthetic colours may cause many side effects to human being. Keeping this in view the present invention is undertaken to develop purely natural herbal colourants for lipstick. This invention also pertains to the development of Herbal Lipstick with mood altering functional attributes including stimulation of creative thoughts on persons who apply the same on lips. These functional attributes are attributed to the selected blended formulations of Natural colours and essential oils/aroma isolates incorporated in these lipstick. Lips being the most sensitive part of skin, can effect fast transdermal absorption and also the lips being very close to nose could facilitate a continuous inhalation of the slowly vaporizing essential oils/aroma chemicals blended in the lipstick, thus, proving a double effect on the specific centers of the brain leading to mood alteration and change of mental perceptions. The different blends of essential oil/aroma isolates/natural aroma chemical selectively blended in the lipsticks give anti-depressant, mood enhancing/ mood lifting and creative thoughts inducing mental state. While the lipsticks with different colour shades blended with aromatic principles is developed for women, another range of lipsticks have also been developed without colours but with a moisturizing transparent type for men to have similar mood altering functions and to achieve altered mental perception similar to that of the lipsticks developed for women. Both the groups of lipstick have some additional health promotive/protective and beautifying attributes by preventing the lips from darkening and providing it with moisturizing effects that give attractive lustre and texture to the lips. The lipsticks with colour, developed for women, has antibacterial, antifungal and anti-inflammatory effects too. With regard to lip beautification, topical application lipstick with different shades of colours are well known. Likewise, spraying of aromatic oils or sprays for refreshing is also well known. Many studies have been carried out on the effect of fragrance on mental perception; for example the nice fragrance has an aesthetic impression and multiple positive effects on our life, they are not only for pleasure and seduction, healing and magic products but also for positive mood creators. Reference may be made to a US patent (No. 5,593,662) wherein moisturizing lipstick has been described. In this invention use has been made with a composition of 30-80% lipophilic material, which may have lesser shelf life and may promote microbial growth due to the presence of moisture. Use has been made of about 0-35% synthetic colours, which seems to be too high. The synthetic colours mostly exhibit harmful side effects like loss of lusture, blackening of skin and may have some carcinogenic effects too as shown in a website (http://www.orst.edU/foodresource/color/colorants/.html. Another reference may be made to US Patent no. 5,665,778 wherein a ceramide, process for their preparation and their application in cosmetics and in dermato pharmacy has been disclosed. These compounds are complex mixture of erythro & three diasterioisomers. Synthesis of these compounds has been done by a complex and costly process. Use has been made of organic pigments for lipstick and there is no mention of herbal colourantss being used. Reference may be made to a recent PCT application (PCT/EPOO/02217 of 13 March 2000) wherein the inventors have used Zinc salts, particularly Zinc citrate in lipstick to effect anti microbial property. The drawback in using Zinc or its salts is that mostly they are emetic and cause conjunctivitis as side effect. Reference is made to an International Congress of Essential oils, fragrance and flavours (November 1989) wherein the description of use of aroma has not at all been mentioned in lipstick. The available lipsticks in the international market are used as refreshing beatifying agents only. Reference is made to yet anther US patent No. 5,858,348 wherein only a single isolate of essential oil like rose oxide, has been used in synthetic lipstick and other cosmetic for refreshing feel. Such a single isolate of essential oil will not serve the desired multiple effects like mood enhancing, sensual pleasure and thought inducing state of mind. To the best of our knowledge there does not exist any lipstick with functional attributes with herbal colours, similarly the cosmaceuticals like eye shadows and glow glitters, rouges with use of herbal colours with the desired characteristics of being safe, health protective, mood enhancing and eco friendly are also not known to be available in any market. The main objective of the present invention relates to a process for preparation of herbal colours useful for cosmaceutical applications. Yet another objective of the present invention is to use the herbal colours in lipsticks. Still another objective of the present invention is to use the herbal colours in other cosmetic purposes like eye shadow, glow glitters, rouges and skin conditioning agents. Yet another objective of the present invention is to provide the use of the functional lipstick as a means to camouflage leucodermic skin and particularly of lips. Another objective of the present invention is the use of herbal colours in hair care products particularly for antidandruff action. Accordingly, the present invention provides a process for the extraction of organic colourants from plant materials, said process comprising the steps of: a) drying the plant parts; b) powdering the dried plant parts; c) subjecting the dry powder obtained in step (b) to Soxhlet extraction at a temperature in the range of 40-80 degree C or cold percolation with organic solvents at a temperature between 20 to 45 degree C; d) concentrating the mixture of step (c) by conventional methods at reduced pressure in the range of 50-100 psi and at a temperature not exceeding 50 degree C; e) mixing the concentrate of step (d) with silica gel in the ratio 1:3 to 2:7 to obtain a slurry; f) eluting the slurry with organic solvents resulting in various fractions; g) concentrating the fractions at a pressure in the range of 50-100 psi resulting in herbal colourants, optionally treating the said colours with acids or bases to produce various shades and; h) obtaining various colours from by treating the said fractions with acids or bases to produce colourants of various shades. An embodiment of the present invention is that the natural source may be selected from a group of plants belonging to the family Boraginaceae. An another embodiment of the present invention, the natural source may be in the form of root, stem and leaf. An another embodiment of the present invention, the dried plant material may be powdered having a size in the range of 30-60 mesh. An another embodiment of the present invention, the plant material may be dried in shade, at a temperature in the range of 30-45° C, An another embodiment of the present invention, the extraction of the plant material may be effected by Soxhlate extraction or by cold percolation method, using non polar solvents or mixtures of non polar and polar solvents preferably hexane, petroleum ether and chloroform. In an another embodiment of the invention, the plant material may be Soxhlated for hot percolation at temperature range of 40 - 80,C. In an another embodiment of the invention, the plant material may be cold percolated at temperature range of 20 - 45 C. In an another embodiment of the invention, the extraction may be carried out with the non polar and mixtures of non polar and polar solvents. In another embodiment the non-polar solvents may be selected from hexane, petroleum ether, toluene and cyclohexane In another embodiment, the polar solvents may be selected from chloroform, acetone, ethyl alcohol and methyl alcohol. In another embodiment, the herbal colours may be obtained by concentrating the extracts at reduced pressure of 50-100 psi and a temperature at a range of 40 - 60°C. In another embodiment the concentrates may result in purplish red, cerise, ruby red, beetroot purple, dark violet, deep blue, and blackish blue colours which are herbal in nature as no trace of organic solvent remains in the final concentrate. An embodiment of invention is that the novel herbal colours may be antimicrobial and anti-inflammatory In an embodiment of the present invention, is that the colour may be changed by treating the said colour with the acid selected from a group consisting of organic acids such as formic acid and acetic acid; inorganic acids such as HCI, HN03 and H2SO4 In another embodiment of the present invention the acid concentration may be in the range of 0.1% -10%. In an embodiment of the present invention, is that the colour may be changed by treating the said colour with the bases selected from a group of organic bases such as sodium acetate, potassium acetate and diethyl amine; inorganic bases such as NaOH, KOH, Na2CO3 and NaCI In another embodiment of the present invention the base concentration is in the range of 0.1% to 20%. The process for extraction of colours from plant materials which comprises drying of plant materials, the dried natural source being powdered by known means, the said dried powder being sieved through mesh to get a powder of particles of a suitable size preferably in the range of 30-60 mesh. The dried powder may then be extracted by Soxhlation at a temperature range of 40-80°C. The dried powdered plant material may also be extracted by cold percolation at a temperature range of 20-45°C. The extraction may be carried out with the non polar and mixtures of non polar and polar solvents selected for the extraction. Non-polar solvents may be selected from hexane, petroleum ether, toluene and cyclohexane whereas the polar solvents may be selected from chloroform, acetone, ethyl alcohol and methyl alcohol. The herbal colours may be obtained by concentrating the extracts at reduced pressure of 50-100 psi and a temperature at range of 40 - 60°C. This process of concentration may result in purplish red, cerise, ruby red, beetroot purple, dark violet, deep blue, and blackish blue colours which are herbal in nature as notrace of organic solvent remains in the final concentrate. The present invention is that the safe herbal colours may be isolated from different plant species belonging to the genus Arnebia, Butea, Hibiscus, Jatropha, Lithospermum, Macrotomia, Maharanga Rhododendron, Onosma and Tagetes which are non-toxic and may be free from any side effects. The herbal colours may extracted from any of the three parts of the plants; namely root, stem or leaves or by taking all of them. These parts may then dried by any conventional means which may include heat treatment at a temperature between 30-450C. Alternatively the drying process may be effected in shade though the time for drying may be rather too long. The dried plant material may then be powdered and sieved through mesh to get a powder of particles of a suitable size preferably in the range of 30-60 mesh These novel colours may be used with or without the aroma isolate/essential oils. The aroma isolates may essentially be selected from group of plants - Aquillaria, Cinnamomum, Cymbopogon, Elettaria, Eucalyptus, Geranium, Pelargonium, Rosa, Rosamarinus, Santalum and Vetiveria. Proper mixture of aroma isolates/essential oils may result in such desirable properties of mood enhancement, sensual pleasure, antidepressant and creative thoughts inducer To get these desired properties in cosmetics like lipsticks the herbal colours may be mixed with selected mixture of aroma and applied to the base material. These herbal colours may be used in other applications like eye shadow, glow glitters, rouges, skin conditioning agent and hair care products. These colours may be the mixture of naphthazarins and may be cyclic unsaturated diketones in which double bonds and keto group may be conjugated. These herbal colours may be changed to different shades by treating it with organic and inorganic acids. The intensity of these colours may be increased with organic acids and may be decreased with inorganic acids. The range of the concentration of the acids may be 0.1-10%. The colour of the herbal colourants may be changed from red to blue with organic and inorganic bases. The range of the concentration of the bases may be 0.1-20%. These herbal colours may have excellent lipophilic properties and very minimum hydrophilic properties. These colours may be soluble in organic solvents like - hexane, petroleum ether, benzene, diethyl ether, ethylacetate, chloroform, acetone and alcohol in the range of 30-100%. The pH of the extracted colours may be within the range of 5-6. All these characteristics of the herbal colours are very desirable for use in cosmaceutical applications A novelty of the present invention is the extraction of the herbal colours from plant materials which are non toxic and highly lipoghilic, A novelty of the present invention lies in application of herbal colours in cosmaceutical preparations like lipsticks, eye shadow, glow glitters and rouges. A further novelty lies in the ability to tailor the shade of the basic herbal colours by a simple treatment of the produce with organic or inorganic acids or bases. The following examples are given to illustrate the invention and should not be construed to limit the scope of the present invention. Examplel 100 gm air-dried coarsely powdered root of Onosma species is sieved in 40 mesh sieve and then extracted in Soxhiet apparatus with hexane at a temperature of 50°C for 12 - 18 hours which resulted in the formation of hexane soluble herbal matter. The said matter was concentrated at a reduced pressure of 70 psi and at a temperature of 35°C, resulting in the yield of 6.0 gm. as the purplish red colour (Plate NO 12 A7 of Methuen handbook of colour, 1978). Example 2 100 gm air dried coarsely powdered stem and root in the ratio of 1: 4 of Onosma species is sieved in 40mesh sieve and then extracted in Soxhiet apparatus, with chloroform, at a temperature of 60°C for 18 - 24 hours which resulted in the formation of chloroform soluble herbal matter. The said matter was concentrated at a reduced pressure of 80 psi and at the temperature of 40°C, resulting in the yield of 8.5 gm. as the beetroot purple (Plate No: 13 D8) Example-3 100 gm air dried coarsely powder stem, root and leaf in the ratio of 1: 1: 3 of Macrotomia species is percolated at room temperature with the mixture of chloroform and hexane in the ratio of 5:95 for 4 hours (3 times). Combined all the extracts and concentrated at a pressure of 70psi and a temperature of 50°C. Thus 3.5 gm of cerise colourant (Plate No: 12 C8) was obtained. Example-4 100 gm air-dried coarsely powdered root of Onosma species is sieved in 40 mesh sieve and then extracted in Soxhlet apparatus with hexane at a temperature of 50°C for 12 - 18 hours which resulted in the formation of hexane soluble herbal matter. The said matter was concentrated at a reduced pressure of 70 psi and at a temperature of 35°C, resulting in the yield of 6.0 gm. as the purplish red colour (Plate NO 12 A7) which gets changed to rose red after treatment with 1% formic acid. Example 5 100 gm air dried coarsely powdered stem and root in the ratio of 1: 4 of Onosma species is sieved in 40mesh sieve and then extracted in Soxhlet apparatus, with chloroform, at a temperature of 60°C for 18 - 24 hours which resulted in the formation of chloroform soluble herbal matter. The said matter was concentrated at a reduced pressure of 80 psi and at the temperature of 40°C, resulting in the yield of 8.5 gm. as the beetroot purple (Plate No: 13 D8) which gets changed with 0.2% HCI to ruby red colour (Plate No: 12 D8). Example-6 100 gm air dried coarsely powder stem, root and leaf in the ratio of 1: 1: 3 of Macrotomia species is percolated at room temperature with the mixture of chloroform and hexane in the ratio of 5:95 for 4 hours (3 times). Combined all the extracts and concentrated at a pressure of 70psi and a temperature of 50°C. Thus 3.5 gm of cerise colour (Plate No: 12 C8) was obtained which gets changed to vivid blue (Plate No: 21 A8) with the addition of the 2% NaOH. Example-7 0.5 mg of herbal colour was mixed with 1 ml of Safflower oil and 1 ml Castor oil thoroughly. In the said mixture 1.5 gm of melted bees wax was mixed at a temperature of 70°C. After that 5 microlitre tocopherol and 1 microlitre of Rosamarinus essential oil was added to the aforesaid mixture. Then the mixture was cooled to room temperature. This cooled mixture is now ready for application. Example-8 0.5 mg of herbal colour was mixed with 1 ml of Safflower oil and 1 ml Castor oil thoroughly. In the said mixture 1.5 gm of melted bees wax was mixed at a temperature of 70°C. After that 5 microlitre tocopherol and 1 microlitre each of Jasminum and Santalum essential oils were added to the aforesaid mixture. Then the mixture was cooled at room temperature. This cooled mixture is now ready for application. Main advantages of the present invnetion are: 1. Herbal colours offer an advantage in that they can be added or used without taking into consideration certification by different agencies like FAO, WHO and Cosmetic authorities etc. 2. The herbal colours are safe, eco-friendly and health protective. 3. These herbal colours may be used in more sensitive and delicate parts of the body like lips, cheeks and eyelids. 4. These herbal colours can be used in leucoderma particularly of lips region. 5. The herbal colours are 100% lipophilic in nature. 6. The herbal colours are antimicrobial, anti-inflammatory and anti dandruff agents. 7. The herbal colours are free from any strong side effects like carcinogenic effects to the users. 8. The herbal colours can be made in different shades in a cost-effective manner. 9. Addition of different essential oil and their isolates promotes the stimulation of creative thoughts, enhance sensual feeling induce positive mental health and well being and to help to overcome the depressant feelings (anti- depressant). We Claim: 1. A process for the extraction of organic colourants from plant materials, said process comprising the steps of: a) drying the plant parts; b) powdering the dried plant parts; c) subjecting the dry powder obtained in step (b) to Soxhlet extraction at a temperature in the range of 40-80 degree C or cold percolation with organic solvents at a temperature between 20 to 45 degree C; d) concentrating the mixture of step (c) by conventional methods at reduced pressure in the range of 50-100 psi and at a temperature not exceeding 50 degree C; e) mixing the concentrate of step (d) with silica gel in the ratio 1:3 to 2:7 to obtain a slurry; f) eluting the slurry with organic solvents by conventional methods resulting in various fractions; g) concentrating the fractions obtained in step [f] at a pressure in the range of 50- 100 psi resulting in herbal colourants, optionally treating the said colours with acids or bases of the kind such as herein described to produce various shades; h) obtaining various colours by treating the said fractions with acids or bases to produce colourants of various shades. 2. A process as claimed in claim 1 wherein, the organic solvent is selected from polar solvents, non-polar solvents or mixtures thereof. 3. A process as claimed in claim 1 wherein, the polar solvents are selected from acetone, chloroform, ethyl acetate, methanol and ethanol. 4. A process as claimed in claim 1 wherein, the non-polar solvents are selected from petroleum ether, hexane, toluene and cyclohexane. 5. A process as claimed in claim 1 wherein, the plants are selected from the group of plants belonging to the family Boraginaceae. 6. A process as claimed in claim 1 wherein, the plant parts are selected from root, stem and leaf. 7. A process as claimed in claim 1 wherein, the plant parts are dried at a temperature in the range of 30-45 degree C in shade. 8. A process as claimed in claim 1 wherein, the dried plant parts are powdered to particle size in the range of 30-60 mesh. 9. A process as claimed in claim 1 wherein, the extraction of the plant material is effected by Soxhlate extraction or by cold percolation method, using non-polar solvents or mixtures of non-polar and polar solvents preferably hexane, petroleum ether and chloroform. 10. A process as claimed in claim 1 wherein, the acid used is selected from the group consisting of organic acids preferably formic acid and acetic acid, inorganic acids preferably HCI, HNO3 and H2SO4. 11. A process as claimed in claim 1 wherein, the acid concentration is in the range of 0.1% to 10%. 12. A process as claimed in claim 1 wherein, the bases are selected from organic bases preferably sodium acetate, potassium acetate and diethyl amine and inorganic bases preferably NaOH, KOH, Na2CO3 and NaCI. 13. A process as claimed in claim 1 wherein, the concentration of the base is in the range of 0.1% to 20%. 14. Herbal colourant shades obtained by a process as claimed in claim 1, wherein the colourants ranges from purplish red, cerise, ruby red, beetroot purple, dark violet, deep blue, blackish blue, pastel red, pale red, purplish red, rose red, cerise, ruby red, deep magenta, beet root purple, amaranth, dark purple, dark violet, deep violet, deep blue and blackish blue. 15. Herbal colourant composition comprising 0.1 to 10.0% of the herbal colourant shades obtained by a process as claimed in claim 1, along with a cosmetically acceptable amount of one or more additives selected from essential oils/aroma and a cosmetically acceptable base material. 16. A process for the extraction of organic colourants from plant materials substantially as herein described with reference to the foregoing examples.

Documents:

143-del-2001-abstract.pdf

143-del-2001-claims.pdf

143-del-2001-correspondence-others.pdf

143-del-2001-correspondence-po.pdf

143-del-2001-description (complete).pdf

143-del-2001-form-1.pdf

143-del-2001-form-19.pdf

143-del-2001-form-2.pdf

143-del-2001-form-3.pdf

143-del-2001-petition-137.pdf

143-del-2001-petition-138.pdf