Title of Invention

A PROCESS FOR PREPARATION OF HERBAL COLOURS USEFUL FOR COSMACEUTICAL APLICATIONS

Abstract

The primary objective of the present invention is to prepare a safe, eco-friendly, health protective and beauty enhancing herbal colours from plants. The herbal safe colours have been developed from different plant species belonging to the genus Arnebia, Jatropha, Lithospermum, Macroiomia, Maharanga, Onosma. Various novel colours were differentially extracted by following certain well-defined extraction methods and these can be changed by treating them with acids or bases. These colours are lipophilic in nature and have antimicrobial and anti-inflammatory properties. These novel herbal colours are highly useful in different cosmaceutical application like lipstick, eye shadow, rouges, and glow glitters. Another important objective of the present invention is to use these colours in lipstick with a medium of aroma therapy in order to get desired effects like mood enhancement, sensual pleasure, anti-depressant and creative thoughts inducer.

Full Text

This invention relates to a process for preparation of herbal colours useful for cosmaceutical application. 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, have antibacterial, antifungal and anti-inflammatory effects too. With regard to lip beautification, topical application lipsticks 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 colourant 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 & threo 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 colourants 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 shadow 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 application. Another objective of the present invention is to use herbal colors in skin conditioning agents. 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 and rouges. Yet another objective of the present invention is to provide the use of functional lipstick as a means to camouflage leucodermic skin and particularly 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 preparation of herbal colours useful for cosmaceutical applications which comprises; drying characterised in that plant material- natural source selected from a group of plants belonging to the family Boraginaceae and powdering by methods such as herein described, percolating said powdered plant materials with alcohol at room temperature resulting in alcohol soluble herbal material, concentrating the alcohol soluble herbal material at a pressure in the range of 50-100 psi and at a temperature in the range of 40-60°C, followed by column chromatography using adsorbent and eluting with mixture of non polar organic solvents and chloroform, resulting in fractions, the said fractions further being concentrated at a pressure in the range of 50-100 psi to give natural colours, optionally treating the said colour with acid or bases to produce various shades. In another embodiment of the present invention , the natural source may be selected from a group of plants belonging to the family of Boraginaceae. In an embodiment of the present invention, natural source may be in the form of root, stem and leaf. In an embodiment of the present invention, the natural source may be dried in shade, at a temperature in the range of 30-45° C, In an embodiment of the present invention the dried natural source may be powder having a size in the range of 30-60 mesh. In an embodiment of the present invention the alcohol used may be selected from group consisting of ethanol and methanol. In an embodiment of the present invention the non polar organic solvents may be selected from a group consisting of hexane, petroleum ether, cyclohexane, toluene. In an embodiment of the present invention the mixture of non-polar solvent to chloroform may be prepared in a ratio in the range of 95: 5 to 25: 75 In an embodiment of the present invention, the colour of the concentrate may be pastel red, pale red, purplish red, rose red, cerise, ruby red, deep magenta, beetroot purple, amaranth, dark purple, dark violet, deep violet, deep blue and blackish blue In an embodiment of the present invention the herbal colour 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, HNO3 and H2S04 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 material, the dried plant material being powdered by known means, the said dried powder being used in percolating with alcohol at room temperature resulting in alcohol soluble herbal material, the said herbal material being concentrated by known means at a pressure in the range of 50-100 psi and at a temperature in the range of 40-60°C, the said concentrate being made into a slurry with silica gel in a ratio in the range of 1:3 to 2:7, the said slurry being eluted by known means with mixture of non polar organic solvents to chloroform, resulting in fractions, the said fractions further being concentrated by known methods at a pressure in the range of 50-100 psi. 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 colourant may be 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 be dried by any convnetional means which may include heat treatment at a temperature between 30-456C. 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 In the process, the dried, powdered plant material may be percolated with ethyl or methyl alcohol at a temperature in the range of 20-48°C. The alcohol soluble matter may be concentrated at reduced pressure of 50-100 psi and at a temperature in the range of 40-60°C. Thus, the said concentrate may be eluted with known column chromatography method. The adsorbent used may be silica gel, neutral alumina or acidic alumina by using non-polar solvents like - hexane, petroleum ether, cyclohexane, toluene and mixture of said non-polar and polar solvents. The polar solvent used may be chloroform, acetone, ethylacetate & methanol. The ratio of the non-polar and polar solvents may be between 95: 5 to 25: 75. The concentration of the column fractions may be made preferably at a pressure in a range of 50 -100 psi and at a temperature in the range of 30-60°C. This process of concentration may result in pastel red, pale red, purplish red, rose red, cerise, ruby red, deep magenta, beetroot purple, amaranth, dark purple, dark violet, deep violet, deep blue and blackish blue colours which are herbal in nature as no trace of organic solvent remains in the final concentrate. These oncentrate are now ready for use with or without the aroma isolates/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. It may be the proper mixture of a few of the aroma species which 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 may be applied to the base material. In other applications, the herbal colours may be used in eye shadow, glow glitters, rouges, skin conditioning agent and hair care products. These novel colours may also be used in leucoderma, more particularly of lips. Further the herbal colours may be used in hair oils as antidandruff agent. The red colourant may be the mixture of naphthazarins and may be cyclic unsaturated diketones in which double bonds and keto group may be conjugated. The red herbal colourants 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 herbal colours may be changed from red to blue with organic and inorganic bases. The herbal colours may have excellent lipophilic properties and very minimum hydrophilic properties. The 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 colourants may be within the range of 5-6. All these characteristics of the herbal colourants 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 lipophilic. 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 percolated with ethyl alcohol at room temperature for 24 hours (4 times). The alcohol soluble portion of stem and root was concentrated at reduced pressure of 70 psi and at a temperature of 50°C, resulting in the formation of 18 gm. of ethanol soluble concentrate. The said concentrate was mixed with 54 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this dried slurry was carried out by using hexane: chloroform in the ratio of 95: 5. The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 90 psi and at a temperature of 40°C, thereby giving the yield of 0.3 gm as the pastel red colour (Plate No:9 A5 of Methuen handbook of colour, 1978). Example 2 100 gm air dried coarsely powder stem and root in the ratio of 1: 4 of Onosma species is percolated with methyl alcohol at room temperature for 24 hours (5 days). The methanol soluble portion of stem and root was concentrated at reduced pressure of 80 psi and at a temperature of 55°C, resulting in the formation of 17 gm of methanol soluble concentrate. The said concentrate was mixed with 52 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this slurry was carried out by using petroleum ether: chloroform in the ratio of 80 : 20. The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 60 psi and at a temperature of 50°C, thereby giving the yield of 1.5 gm as the ruby red colour (Plate No: 12 D8). Example-3 100 gm air dried coarsely powder stem, root and leaf in the ratio of 1: 1: 3 of Onosma species is percolated with methyl alcohol at room temperature for 24 hours (5 days). The methanol soluble portion was concentrated at reduced pressure of 60 psi and at a temperature of 50°C, resulting in the formation of 16.5 gm of methanol soluble concentrate. The said concentrate was mixed with 50 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this slurry was carried out by using petroleum ether : chloroform in the ratio of 1 : 1 The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 70 psi and at a temperature of 50°C, thereby giving the yield of 1.5 gm as the blackish blue colourant (Plate No: 18 F8). Example-4 100 gm air dried coarsely powder stem, root and leaf in the ratio of 1: 1: 3 of Onosma species is percolated with methyl alcohol at room temperature for 24 hours (5 days). The methanol soluble portion was concentrated at reduced pressure of 60 psi and at a temperature of 50°C, resulting in the formation of 16.5 gm of methanol soluble concentrate. The said concentrate was mixed with 50 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this slurry was carried out by using petroleum ether: chloroform in the ratio of 80: 20 The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 70 psi and at a temperature of 50°C, thereby giving the yield of 1.5 gm as the ruby red colourant (Plate No: 12 D8) which gets changed to rose red after treatment with 1% formic acid. Example-5 100 gm air dried coarsely powder root and leaf in the ratio of 4: 1 of Onosma species is percolated with methyl alcohol at room temperature for 24 hours (5 days). The methanol soluble portion was concentrated at reduced pressure of 60 psi and at a temperature of 50°C, resulting in the formation of 17 gm of methanol soluble concentrate. The said concentrate was mixed with 50 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this slurry was carried out by using petroleum ether: chloroform in the ratio of 1 : 1 The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 80 psi and at a temperature of 50°C, thereby giving the yield of 1.5 gm as the blackish blue colourant (Plate No: 18 F8) which gets changed with 0.2% HCI to deep blue colour (Plate No: 21 D8). Example-6 100 gm air dried coarsely powdered root of Onosma species is percolated with ethyl alcohol at room temperature for 24 hours (4 times). The alcohol soluble portion of stem and root was concentrated at reduced pressure of 70 psi and at a temperature of 50°C, resulting in the formation of 18 gm. of ethanol soluble concentrate. The said concentrate was mixed with 54 gm of silica gel for preparing slurry. This slurry was dried with the help of vacuum pump. The column chromatography of this dried slurry was carried out by using hexane: chloroform in the ratio of 95: 5. The fractions obtained with aforesaid solvents were concentrated at the reduced pressure of 90 psi and at a temperature of 40°C, thereby giving the yield of 0.3 gm as the pastel red colour (Plate No:9 A5) which gets changed to vivid blue ( Plate No: 21 A8) with the addition of the 2% NaOH. Example-7 0.5 mg of rose red colourant was mixed with 1 ml of Sapflower 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 deep blue colourant was mixed with 1 ml of Sapflower 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 to 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 oils 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 preparation of herbal colours useful for cosmaceutical applications which comprises; drying characterised in that plant material- natural source selected from a group of plants belonging to the family Boraginaceae and powdering by methods such as herein described, percolating said powdered plant materials with alcohol at room temperature resulting in alcohol soluble herbal material, concentrating the alcohol soluble herbal material at a pressure in the range of 50-100 psi and at a temperature in the range of 40-60°C, followed by column chromatography using adsorbent and eluting with mixture of non polar organic solvents and chloroform, resulting in fractions, the said fractions further being concentrated at a pressure in the range of 50-100 psi to give natural colours, optionally treating the said colour with acid or bases to produce various shades. 2. A process as claimed in claim 1 wherein, natural source is in the form of root, stem and leaf. 3. A process as claimed in claim 1 - 2 wherein, the natural source is dried in shade, at a temperature in the range of 30-45°C. 4. A process as claimed in claims 1-3 wherein the dried natural source is powder having a size in the range of 30-60 mesh. 5. A process as claimed in claims 1-4 wherein the alcohol used is selected from group consisting of ethanol and methanol. 6. A process as claimed in claims 1-5 wherein the non polar organic solvents are selected from a group consisting of hexane, petroleum ether, cyclohexane, toluene. 7. A process as claimed in claims 1-6 wherein the mixture of non-polar solvent to chloroform is prepared in a ratio in the range of 95:5 to 25:75. 8. A process as claimed in claims 1-7 wherein the said acid used is selected from a group consisting of organic acids such as formic acid and acetic acid, inorganic acids selected from HCL, HNO3 and H2SO4 9. A process as claimed in claims 1-8 wherein, the said acid concentration is in the range of 0.1%-10%. 10. A process as claimed in claims 1-9 wherein said bases used are selected from organic bases such as sodium acetate, potassium acetate and diethyl amine and inorganic bases such as NaOH, KOH, Na2CO3 and NaCl 11. A process as claimed in claims 1-10 wherein the said base concentration is in the range of 0.1% to 20%. 12. A process for preparation of herbal colours useful for cosmaceutical applications substantially as herein described with reference to the examples in this specification.

Documents:

144-del-2001-abstract.pdf

144-del-2001-claims.pdf

144-del-2001-correspondence-others.pdf

144-del-2001-correspondence-po.pdf

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

144-del-2001-form-1.pdf

144-del-2001-form-19.pdf

144-del-2001-form-2.pdf

144-del-2001-form-3.pdf