Title of Invention

A PROCESS FOR PREPARATION OF WATER DISPESIBLE CAROTENOID

Abstract

Water dispersible carotenoid formulations and preparation thereof. Water-dispersible carotenoid formulations are prepared by adding finely pulverized carotenoid powder to a water dispersible matrix to which an antioxidant namely ascorbic acid is added, following which the dry blended powder is coated with edible oil using a suitable blender would thus obtain a powder which will evenly disperse in water at room 35 deg C. The produce can be used for coloring foods and is stable to creaming. The produce can be used for dry filling in hard gelatin capsules or can be granulated for tablet use.

Full Text

"i he present invention relates to water dispersible carotenoid formulations and process for preparation thereof It is an object of the present invention to provide a protective colloid, imparts all the required properties to the carotene formulation. PRIOR ART: The colors of a large number of plants and animals are determined by substances belonging to the carotenoid group. These are compounds which have intense yellow to red colors The most important members of the two classes are Beta-carotene, canthaxanthin, citranaxanthin, Beta.-apo-8*-carotenal and esters of Beta.-apo-8'-carotenic acid. These carotenoids are not harmful to health and in some cases even have a health-promoting provitamin A action, these compounds are increasingly being used as colorants or additives for food, drugs, cosmetics and animal feeds. While oily or fatty systems can be fairly readily colored with the pure crystalline substances, aqueous systems are virtually impossible to color with the substances. Furthermore, pure carotenoids mixed with food or animal feed are poorly utilized by the human or animal organism. The reason for this is the complete insolubility of most carotenoids in water. The carotenoids have only very limited solubility even in organic solvents such as alcohols and alkanes. U.S. Pat. No. 2,861,891 describes a process for the preparation of water-dispersible carotene formulations. In this process the carotenoid, eg. Beta-carotene as one of the most important members of this group, is dissolved in a vegetable oil at elevated temperatures, this oil solution is emulsified in an aqueous protective colloid system and the resulting emulsion is converted to a dry powder by removal of water. References Cited: U.S. Patent Documents: 2861891 Nov., 1958 Bauemfeind et al. 426/540. 3110598 . Nov., 1963 Muller et al. 426/540. 3125451 Mar., 1964 Wingerdetal. 426/540. 3206316 Sep., 1965 Klaui 426/540. 3316101 Apr., 1967 Borenstein et al. 426/540.. 3655406 Apr., 1972 Klaui 426/540. 3998753 Dec, 1976 Antoshkiw et al. 426/540. 4522743 Jun., 1985 Horn et al. 426/540. Foreign Patent Documents: 50-75215 Jun., 1975 JP 426/540. Other References: H. Klaui, Wiss. Veroffentl. Deutsch. Ges. f. Emahrung 9, (1963), p. 396. If the dry powder is redispersed in warm water, a cloudy, orange yellow emulsion is formed again. This can be used, for example, for coloring foods. Important performance characteristics of these coloring formulations are solubility, hue, color strength, turbidity and stability in the medium used. Good solubility in cold water, an intense yellow hue, a low level of turbidity and high stability even in acidic solution (2 Conventionally some of these properties are obtained by using gum arabic as a protective colloid in the aqueous phase. However, the use of gum arabic in a food additive has recently presented very great problems since the quality varies very greatly and moreover the microbiological status of this natural product, which accumulates in the human body, does not meet the requirements of quality-conscious food producers. Field of Invention: The object of the present invention is to provide a protective colloid, imparts // all the required properties to the carotene formulation. A process for the preparation of finely divided carotenoid dispersions having high color strength, and of carotenoid-containing dry powders which are obtained from these dispersions are, dispersible in cold water, using a mixture of an edible oil and, a starch product which is soluble in cold water. According to the present invention, a process for the preparation of a water-dispersible carotenoid formulation by dispersing a finely divided Betacarotene crystal in a colloid matrix namely a dextrin to which ascorbic acid is added to stabilize the carotenoid and finally dispersed in oil which is soluble in cold water. Dextrin is a partially hydrolyzed starch which is obtained, either by means of heat alone or heat in the presence of an acid, from various starches (com starch, potato starch, wheat starch, rice starch etc.), as described in, for example, "Food Chemical Codex", third edition 1981, National Academy Press, page 96, or "Starch: Chemistry and Technology", Academic Press, Inc. (1984), second edition. which are herein incorporated by reference. The degree of hydrolysis is generally stated as dextrose equivalent (DE). It is a measure of the amount of reducing sugar, calculated as D-glucose and based on dry weight. The DE value is the reciprocal of the degree of polymerization. Unhydrolyzed starch has a DE value of virtually' 0, while, in conformity with the definition, C-glucose has a DE value of 100. Suitable dextrin has, for example, a DE value of less than 20, preferably from 1 to 8. The ratio of the said cold water-soluble starch product to the edible oil is 1:50 to 1:30. The edible oil used contains as a rule predominantly Cig to C20 fatty acids. DETAIL DESCRIPTION OF THE INVENTION: The carotenoid is dispersed initially in dextrin and finely dispersed using multiple rollermill. This step is followed with the addition of edible oil and the dispersion is achieved by using a muller mixer. The mixing operation is performed for a period of six minutes. This renders the product disperse in cold water. Examples of suitable vegetable oils are sunflower oil, orange peel oil, soya bean oil, cotton seed oil and peanut oil. The concentration of the carotenoid in the dextrin is from the 10 to 20 % by weight, and sometimes 30 %. The carotenoid should be milled so that the resuhing particle size distribution substantially excludes crystals >10 .mu.m. This ensures uniform solution kinetics. The minimum drop size obtainable by these measures is dependent on the type of emulsifying apparatus, the formulation and the duration of emulsification. If a dispersing apparatus functioning on the principle of the rotor-stator is used and the preferred ratio of starting materials is chosen, a mean particle size of 0.3 .mu.m .+-.50% is obtained. This is unusually low for an OAV emulsion and is very advantageous with regard to the end product since both color strength and hue and turbidity are shijfted in the stated advantageous direction as the droplets become smaller. The particle size is measured by photon correlation spectroscopy, as for the choice of the dextrins. The resulting emulsion has a long shelf life and can either be used directly for coloring foods, if necessary with the addition of preservatives, or be subjected to a known process for removing water under mild conditions, for example by spray drying, and then converted to a dry powder which has the special properties stated at the outset. EXAMPLE 1: 700 g of dextrin with an initial moisture content of 5-7%, lOg of ascorbic acid, 265g of mixed carotenoid crystals containing not less than 20% Betacarotene as final concentration is dry blended initially and dispersed uniformly using a multiple rollermill. The product thus obtained is then mixed with 25riil of edible oil and finally milled and mixed using a muller mixer. The Betacarotene used for the formulation has a micron size of 3 microns and below. The resultant formulation is a relatively dry blend which evenly disperses in water and has coloring properties with a less cloud. The oil coating on the colloid gives it long shelf life. The product thus formulated does not contain water, lecithin or gum Arabic thereby is very safe fi'om degradation. The product is suitable for direct filling to hard gelatin capsules or can be granulated successfully. Since the product is devoid of sugar the product is safe for use for patients suffering from diabetics. All the processes are performed under room temperature conditions and under ultrapure nitrogen giving a fomiulation of high stability. We claim, 1. The process for preparation of water dispersible carotenoid formulation comprising; (a) dispersing carotenoid in dextrin and finely milling using multiple roUermiller; (b) stabilizing it using an anti oxidant suitably ascorbic acid; (c) coating with the protective layer consisting of edible oil containing a fatty acid of 18 carbon atoms and a cold water soluble starch product in the weight ratio of 1 : 50 to 1:30. 2. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein edible oil added is sunflower oil. 3. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein dextrin or chemically modified starch is the cold water soluble starch product. 4. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein the starch product is dextrin. 5. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein the carotenoid is Beta-carotene and the starch product is dextrin. 6. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein the blending equipment used for the purpose is a muller mixer. 7. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein the carotenoid crystal size is predominantly 3 microns. 8. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein the formulation is prepared in absence of water. 9. A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein formulation is sugar free. 10.A process for preparation of water dispersible carotenoid formulation as claimed in claim 1 wherein lecithin or gum Arabic are excluded in the formulation. 11. A process for preparation thereof as claimed in claim 1 to 10 as substantially herein described with foregoing description and examples.

Documents:

394-che-2003 claims duplicate.pdf

394-che-2003 abstract duplicate.pdf

394-che-2003 description (complete) duplicate.pdf

394-che-2003-abstract.pdf

394-che-2003-claims.pdf

394-che-2003-correspondnece-others.pdf

394-che-2003-correspondnece-po.pdf

394-che-2003-description(complete).pdf

394-che-2003-form 1.pdf

394-che-2003-form 26.pdf

394-che-2003-form 3.pdf

394-che-2003-form 5.pdf

394-che-2003-form 8.pdf