Title of Invention | A PROCESS FOR THE PREPARATION OF WATER SOLUBLE TURMERIC COLOURANT FORMULATIONS USEFUL AS YELLOW COLOURANT IN FOODS AND BEVERAGES. |
---|---|
Abstract | The present invention provides an improved method for the preparation of 4-t-butylcyclohexyl acetate comprising the steps of: reacting 4-t-butylcyclohexanol with acetylating agent selected from acetic anhydride and acetic acid in the mole ratio in the range of 1:10-1:20; and refluxing the above reaction mixture with 2-10 ml of solvent selected from pyridine at a temperature in the range of 100 - 115 deg C for a period of 2-6 hours characterized in that the said refluxing is carried out in the presence of an additive selected from the group consisting of beta cyclodextrine, DM beta-CD, HP beta-CD epichlorohydrin polymer and covering the product by known methods. |
Full Text | The present invention relates to a process for the preparation of water soluble turmeric colorant formulations useful as yellow colorant in foods and beverages Mjore particularly present invention relates to the A process for the preparation of water soluble turmeric colorant formulations from Curcumin Removed Turmeric Oleoresin useful as yellow colorant in foods and beverages The significance of the new process and the products lies in that the water-soluble turmeric colorant formulations are prepared from Curcumin Enriched Colorant or from pure curcumin using permitted food additives. The CEC is obtained from an industrial waste, viz., Curcumin Removed Turmeric Oleoresin. Curcumin Removed Turmewric Oleoresin, (hereafter mentioned in this document as CRTO), is the mother liquor remaining after separating the recoverable curcumin from turmeric oleoresin, a commercial product of the spice oleoresin industry. The curcumin content in this material is usually between 10-20 % which is not easily isolable with the existing procedures. In order to utilise this by-product which is having a considerable amount of Curcumin in it, the present study was undertaken. Therefore it was decided to prepare the Curcumin Enriched colorant (Hereafter called in this document as CEC), which can be useful in the preparation of water soluble curcumin formulations which can readily dissolve/disperse into water. Hence methods were standardised and concentrations were optimised. Curcumin is a natural dye extracted from the rhizomes of Curcuma longa (Zingiberaceae) and is widely used as a colouring agent in food, drugs and cosmetics. Curcumin is also reported to have various pharmacological effects. It is useful as a natural yellow colorant for food in oil and aqueous media. Curcuma extracts contain three different diaryl heptanoids viz, Curcumin, demethoxy curcumin and bisdemethoxycurcumin. Curcumin is usually the main constituent. In rare cases the other two amount to nearly 70% of the total curcuminoids. Commecrcially available 'pure' Curcumin consists of mixture of the three naturally occurring curcuminoids with curcumin as the main constituent. It is known that curcumin is almost insoluble in water, but soluble in alkali or glacial acetic acid. In solutions at pH 1-7 the colour is yellow and in pH range 7-9 the colour is brownish-red or deep red. Therefore it was decided to prepare the water soluble turmeric colorant formulations which can readily disperse into water so that it can effectively be used in different foods and beverages. Hence methods were standardised and concentrations were optimised. Reference may be made to the US patent No.US 4263333 (1981) entitled 'Curcumin -metal colour complexes' wherein the preparation of a water soluble complex formed from curcumin using metal complexes for use in foods was described. The drawbacks are the toxicity of metals at higher intakes. Further, references may be made to two more patents namely, UK-GB2 13 2205A (1984) entitled 'Colouring agents' wherein the preparation of a water-soluble curcumin complex using source of curcumin and gelatin in acetic acid for food applications was revealed and an US patent No. US4368208 (1983) entitled 'Water soluble curcumin' wherein the method for preparing a water- soluble curcumin - gelatin complex colouring agent for foods was described. The drawback is the use of gelatin and acetic acid in the formulation. In addition to this, reference can be made to the US patent No. US 4999205 (1991) entitled 'a curcumin complex with a water-soluble branched chain or cyclic polysaccharide or a water-soluble or a water dispersible protein was described. The drawbacks are it involves the use of acids/bases for altering the pH. The main object of the present invention is utilisation of the industrial waste, CRTO, which presently does not have any use and to provide a process for the preparation of Curcumin enriched Colorant from Curcumin Removed Turmeric oleoresin and separation of turmeric oil which comes out as a by-product and also a method for the preparation of water soluble turmeric colorant formulations in liquid and powder form and their use as colorant in foods and beverages using CEC, curcumin and permitted food additives, which obviates the drawbacks as detailed above. Accordingly, a process for the preparation of water soluble turmeric colorant formulations useful as yellow colorant in foods and beverages which comprises , a. providing Curcumin Removed Turmeric Oleoresin in a suitable container, b. adding an organic non-polar solvent selected from acyclic and cyclic alkanes in the ratio ranging between 1:5 to 1:2 , c. stirring the above reaction mixture vigorously for 1-4 h at 10 to 30 o C, d. decanting the supernatant and filtering the precipitate followed by washing with the same solvent, e. drying the material and placing the precipitate in a vacuum desiccator using a desiccants to remove the residual solvent and moisture to obtain the product called Curcumin Enriched Cqorant (CEC) as yellowish brown in colour and a free flowing powder, f. mixing the Cucumin Enriched Colorant powder with propylene glycol in the ratio of 1-10 parts to form a paste, g) adding a non ionic surfactant selected from polyoxyethylene, sorbitan mono oleate etc., to the above said paste in the ratio of 1:2 to 1:6 and stirring for 2-5 hours to get a water soluble deep-red viscous liquid formulation with curcumin content of 5-15 percent; and converting the above said liquid formulation into powder form by mixing a carbohydrate monomer/polymer selected from glucose, maltose, starch etc., in the ratio of about 1:2(w/w) followed by drying in a desiccators using desiccant selected from group consisting of P2O5 and anhydrous CaCL2 in order to get the said water soluble turmeric colorant formulation powder useful in foods and beverages as natural yellow colorant with curcumin content of 1-4%. In an embodiment of the present invention, the desiccant used is selected from the group consisting of paraffin wax, phosphorous pentoxide and anhydrous calcium chloride. In an embodiment of the present invention, water-soluble turmeric colorant formulation obtained is useful as natural colorant in liquid as well as solid colorant in various foods. In an embodiment of the present invention, water soluble turmeric colorant formulation obtained as the following characteristic features: (a) liquid formulations are deep reddish brown in color, readily soluble or dispersible in water; and (b) solid formulations are free-flowing bright reddish orange colored, readily soluble or dispersible in water. In an embodiment of the present invention, organic non-polar solvent used is added preferably in the ratio at the range of 1:1 to 1:3 followed by stirring the reaction preferably for 1-3 hours at 15-25 deg C. In an embodiment of the present invention, propylene glycol used is added in the ratio preferably at the ratio of 1:5 (part/part) In an embodiment of the present invention the adding a non-ionic surfactant preferably in the ratio (colorant: non-ionic surfactant, 1:3) Polyoxyethylene (20) sorbitan mono-oleate (PSM) stirred preferably for 2 -3 h. to get a viscous liquid of deep red colour which is water soluble liquid formulation with curcumin content 7-12 %. In an embodiment of the present invention the formulations prepared is used as food colorant in food products like milk, ice creams savouries, bakery-products, snacks (including extruded products), deserts, beverages and confectionery. To determine the curcumin content a standard method of measuring absorbance with UV spectrophotmeter at 425 nm was used. The liquid formulation (L-l or L-2) 0.1 ml was diluted to 10,000 times or as required for recording absorbance, with ethanol and the absorbance (UV) was measured. Based on this , the curcumin content was calculated in L-l and L-2, and was found out to be 5-10% and 3 - 4.5% respectively. These formulations, when added to water (25mg in 20ml), give a clear solution of pleasing yellow colour. The novelty of the new process and the products is that CEC (Curcumin Enriched Colorant) which is obtained from the industrial waste viz., CRTO is converted into water-soluble formulations in liquid and powder forms useful as yellow colorants in foods and beverages. Besides this, turmeric oil is obtained as a by-product during the preparation of CEO from CRTO and the oil is reportedly possessing biological and other applications. The following examples are given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention. Example-1 The CRTO, a gummy substance and an industrial waste, (1 Kg) taken in a stainless steel vessel and 2L of a nonpolar organic solvent, alkane, was added and stirred for 2 h. The volatile oil as well as the fixed oil from the CRTO got dissolved in the solvent and the precipitate having dull yellow brownish colour was separated. The supernatant was decanted and the residue filtered and thoroughly washed with the solvent. The residue was air dried and then kept in a vacuum desiccator over P2O5 and Paraffin wax to remove the residual solvent and moisture present in it. The resultant product, called as Curcumin Enriched Colorant powder, is free flowing in nature and brownish - yellow in colour (yield, 50-60 %). Example 2 CEC powder 10 gm was taken and 15 gm of propylene glycol was added and made into paste. 20 gm of Polyoxyethylene (20) sorbitan mono-oleate a non-ionic surfactant was added and stirred for 5 h to get a viscous liquid of deep red colour i.e., water soluble liquid formulation (L-l). The curcumin content in this formulation was found to be 10%. Example 3 Pure curcumin, 1 part, (95 % pure) was mixed with 2-25 parts of propylene glycol made into a paste to which 10-50 parts of a non-ionic surfactants like Polyoxyethylene (20) sorbitan mono-oleate (PSM) or polyoxyethylene (20)sorbitan monopalmitate was added and stirred for 2 -5 h. to get a clear solution of deep red colour i.e.water soluble liquid formulation (L-2) from pure curcumin with curcumin content 2-5% Example-4 The above formulation (LI or L2, 10 gm) was mixed with Glucose (dried, 20 gm), and the impregnated solid dried in dessicator to get solid formulation (P-l and P-2). The curcumin content in the formulation was found to be 4% and 3.5 %. Example -5 Lemon juice (75 ml) obtained from fresh fruits of lemon was taken in a beaker and added 2 L of water. To this 200 g of Sugar was added and stirred. 25 mg of L-l was added to 2 L of beverage and stirred well. The product was subjected to sensory evaluation for the colorant suitability and found to be satisfactory. The main advantages of the present invention are: 1. An industrial waste product (CRTO) is being utilised in the preparation of the Curcumin Enriched Colorant powder (Yield, 50-60 %). 2. The turmeric oil is obtained as by-product (yield (40-50 %). 3. The formulations are prepared using permitted food additives and are odour free. 4.The formulations described are useful as yellow colorants in ice creams, bakery- products, snacks (including extruded products), desserts, beverages and confectionery. 5. The amount of formulation required to obtain pleasing yellow colour for various food products is at ppm levels. We claim: 1. An process for the preparation water soluble turmeric colorant formulations useful as yellow colorant in foods and beverages, which comprises the steps of: (a) providing curcumin removed turmeric oleoresin in a suitable container; (b) adding an organic polar solvent acyclic and cyclic alkanes selected from methane, ethane, cyclobutane etc., in the ratio ranging from 1:1 to 1:5; (c) stirring the above reaction mixture vigorously for 1-4 hours at 10 - 30 deg C; (d) decanting the supernatant and filtering the precipitate followed by washing with the same solvent; (e) drying the material and placing the precipitate in a vacuum dessicator using dessicants to remove the residual solvent and moisture to obtain Curcumin Enriched Colorant (CEC) in form of free flowing yellow colored powder; (f) mixing the Curcumin Enriched Colorant (CEC) powder with propylene glycol in the ratio of 1:10 (by parts) to obtain a paste; (g) adding a non ionic surfactant selected from polyoxyethylene, sorbitan mono oleate etc., to the above said paste in the ratio of 1:2 to 1:6 and stirring for 2-5 hours to get a water soluble deep-red viscous liquid formulation with curcumin content of 5-15 percent; and (h) converting the above said liquid formulation into powder form by mixing a carbohydrate monomer/polymer selected from glucose, maltose, starch etc., in the ratio of about 1:2(w/w) followed by drying in a desiccators using desiccant selected from group consisting of P2Os and anhydrous CaCL2 in order to get the said water soluble turmeric colorant formulation powder useful as natural yellow colorant in foods and beverages. 2. A process as claimed in claim 1, wherein water-soluble turmeric colorant formulation obtained has curcumin content in the range of 1 -4 percent. 3. A process as claimed in claim 1, wherein water-soluble turmeric colorant formulation obtained is useful as natural colorant in liquid as well as solid formulations. 4. A process as claimed in claim 1, wherein the desiccant used is selected from the group consisting of paraffin wax, phosphorous pentoxide and anhydrous calcium chloride. 5. A process as claimed in claim 1, wherein water soluble turmeric colorant formulation obtained as the following characteristic features: (a)liquid formulations are deep reddish brown in color, readily soluble or dispersible in water; and (b) solid formulations are free-flowing bright reddish orange colored, readily soluble or dispersible in water. 6. A process as claimed in claim 1, wherein organic non-polar solvent used is added preferably in the ratio at the range of 1:1 to 1:3 followed by stirring the reaction preferably for 1-3 hours at 15-25 deg C. 7. A process as claimed in claim 1, wherein propylene glycol used is added in the ratio preferably at the ratio of 1:5 (part/part). 8. A process as claimed in claim 1, wherein non ionic surfactant used is preferably in the ratio of 1:3 and stirred for 2-3 hours to get a water soluble deep-red viscous liquid formulation with curcumin content of 7-12 percent. 9. A process as claimed in claim 1, wherein the water-soluble turmeric colorant formulation obtained is useful as natural colorant in various foods selected from milk, ice creams, savories, bakery products deserts, confectioneries etc., 10. A process as claimed in claim 1, wherein the water-soluble turmeric colorant formulation obtained is useful as natural colorant in various beverages selected from the group consisting of 11. An improved method for the preparation of 4-t-butylcyclohexyl acetate substantially as herein described in description and exemplified in accompanying examples. |
---|
401-del-2001-correspondence-others.pdf
401-del-2001-correspondence-po.pdf
401-del-2001-description (complete).pdf
Patent Number | 230571 | |||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Indian Patent Application Number | 401/DEL/2001 | |||||||||||||||
PG Journal Number | 11/2009 | |||||||||||||||
Publication Date | 13-Mar-2009 | |||||||||||||||
Grant Date | 27-Feb-2009 | |||||||||||||||
Date of Filing | 29-Mar-2001 | |||||||||||||||
Name of Patentee | COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH | |||||||||||||||
Applicant Address | RAFI MARG, NEW DELHI-110 001, INDIA. | |||||||||||||||
Inventors:
|
||||||||||||||||
PCT International Classification Number | A23L 0001/27 | |||||||||||||||
PCT International Application Number | N/A | |||||||||||||||
PCT International Filing date | ||||||||||||||||
PCT Conventions:
|