A method of obtaining a substance based on chitosan for food and pharmaceutical industry

 

(57) Abstract:

The invention relates to biochemical technologies to obtain a gel-like substance for food and cosmetic products based on chitosan. Can be used in medicine, cosmetics and food industry. The method includes preparation of chitosan solution in hydrochloric or acetic acid. Then remove any insoluble particles of chitosan by filtration or sedimentation. Modification of chitosan spend allermuir agent under alkaline conditions at pH 7.0 and 9.0. The obtained pH-neutral substance washed. As Alliluyeva agent use dichlorohydrin dicarboxylic acid. The reaction is carried out at a temperature of 18-25C. to obtain a gel-like product. The weight ratio of dichlorohydrin dicarboxylic acid and chitosan in terms of dry weight is 1:5-1:25. The substance of chitosan-based autoclave or dried by lyophilization, or it is injected organic acids or products of microbiological synthesis, containing organic acids. The method allows to obtain a substance suitable for use in the food and pharmaceutical industries with preservation of biologically active t is aznoe substance for food and cosmetic products based on chitosan and can be used in medicine, the cosmetics and food industry.

In the production of food and medical-cosmetic products find wide application of various biologically active substances such as animal and vegetable origin. Activating the metabolism, improving the physiological condition of the skin when applied externally and immune status of the organism when administered as a dietary Supplement.

Poly-polysaccharide chitosan, a product of the deacetylation of chitin, is widely used in various industries, biotechnology, medicine and cosmetics. Detection of bio-and wound-healing action of chitosan contributed to the creation of new ways of getting defensive and protivorakovykh coatings and methods of making preparations for skin care, such as Survey information products based on chitosan. M., 1987.- C. 2-7) [1].

A method of obtaining the gel based on chitosan by treating chitin alcohol solution containing acetic anhydride, the anhydride of propionic acid or butyric acid anhydride in the amount of 0.5 mole per chitin at a temperature of 30oC for more than 30 min (Japan's Bid N 5-1282, MKI C 08 B 37/12, SDA is, is then obtained on the basis of the product cannot be used as the basis for food or medical preparations, such as ointments, pastes and gels, because it is hard neoplastica structure and is mainly used for chromatography and immobilization of enzymes.

A method of obtaining the gel based on chitosan, comprising preparing a solution of chitosan in dilute acid, mixing the resulting solution with a hydrophobic substance, stirring the mixture to obtain an emulsion, carrying out the reaction of covalent fixation of chitosan in the composition of the emulsion by introducing into it a bifunctional reagent capable of forming covalent cross-linking between molecules of chitosan with subsequent washing and filtering of the received product (ed. mon. USSR N 827492, MKI C 08 B 37/08, publ. 07.05.81 year). The product of this technology is cross-linked gel based on chitosan, representing rigid resulting granules used in chromatography.

The disadvantage of this technical solution is that obtained in this way hard microgranular gels based on chitosan are an inappropriate basis for medical or cosmetic preparations, e.g. yaytsa body. In addition, the use of technology poisonous organic solvents and bifunctional reagents bearing such active groups, as diisocyanate, bisepoxy etc. excludes the use of the products obtained in these areas.

The closest technical solution (prototype) is a method of obtaining derivatives of chitosan in the form of gel for the pharmaceutical industry (patent USSR N 508212, IPC C 08 B 37/08, publ. 04.05.76 year). The method includes preparation of chitosan solution, removing nerastvorim particles of chitosan by filtration or centrifugation and carrying out modifications of chitosan allerease agents under alkaline conditions at pH 7.0 and 9.0 with the subsequent laundering of the finished product, which is released in the form of acid, and in this form he used in the industry. As alleluya agents use unsaturated or saturated anhydrides of dicarboxylic acids of different inner structure of the amino groups of chitosan, such as unsaturated anhydride using maleic, itacademy or citraconic anhydride and a saturated amber, acetoxystyrene, mutilatory, diacetylenic or diglycolic anhydride.

However, the PNA change their charge on the opposite or at least, lose their charge, and with it lost many biologically active properties of chitosan as poly-polysaccharide. In addition, in the description of this technical solution, there are no data about organoplastic characteristics of the gel.

Object of the present invention is to provide such a method which would ensure obtaining a gel-like product on the basis of chitosan with preservation of its biologically active properties as poly-polysaccharide can be used to create immunostimulatory food products and supplements, cosmetic products for skin care, for the treatment or prevention of skin diseases, and hygiene products to care for your mouth.

This task is solved in that in the method of obtaining a substance based on chitosan for food and pharmaceutical industry, including the preparation of a solution of chitosan in dilute hydrochloric or acetic acid, removing nerastvorim particles of chitosan by filtration or sedimentation and carrying out modifications of chitosan allermuir agent under alkaline conditions at pH 7.0 and 9.0 with the subsequent laundering of the obtained pH-matrilineality, the reaction is carried out at a temperature of 18-25oC before the formation of the gel structure of the product when the weight ratio of dichlorohydrin dicarboxylic acid and chitosan in terms of dry weight of 1:5-1: 25, and the resulting pH-neutral substance chitosan-based autoclave, or dried by lyophilization, or it is injected organic acid, or the products of microbiological synthesis, containing organic acid in a quantity sufficient to get ready gel-like substance with a pH of not more than 6.0.

As dichlorohydrin dicarboxylic acid used dichlorohydrin succinic acid, or dichlorohydrin glutaric acid, or dichlorohydrin adipic acid, or dichlorohydrin fumaric acid.

As organic acids using formic or acetic acid, or benzoic acid, or salicylic acid, or aspirin, or glycol, or nicotine, or deoxybenzoin, or lactic acid in an amount of 0.1 to 5.0% relative to the total weight of the final product.

As products of microbiological synthesis, containing organic acids using biomass lactic acid bacteria, Bifidobacterium bifidum or Bifidobacterium longum or Lactobacillus acidophilus or Siva is Ino the total mass of the final product.

Chitosan - acylation product of chitin, which represents a polysaccharide containing polymer chain consisting of glucosamine units.

In the proposed method for the modification of chitosan with the aim of obtaining the gel and pH-neutral substances used as alleluya agents anhydrides (in the prototype), and halides of dicarboxylic acids. This leads to the emergence of another new type of units in the molecules of chitosan, when the molecule dichlorohydrin interacts with both the amino groups located in different parts of the coiled tangle molecules of chitosan or in different molecules. In such relationships can participate from 1 to 50% of the amino groups. The resulting intermolecular bridges form a flexible, movable spatial grid chitosan gel. When this acidic properties of the gel does not occur, i.e., retains all the properties of chitosan as poly-polysaccharide, and the finished product has a highly gelatinous mass.

The difference of the proposed method of obtaining product on the basis of chitosan from known technologies (including the prototype) is that, on the one hand, this method provides receiving plastic gel copper is aznoe basis. This is provided by the fact that the reaction used anhydrides of dicarboxylic acids with chitosan does not form toxic reaction products. On the other hand, the product based on the proposed technology preserves all useful biologically active properties of chitosan as poly-polysaccharide. Moreover, when forming a gel-like substance use components (organic acids and the products of microbiological synthesis) that extend the range of useful biologically active properties of the final product.

Example 1.

Technology of production of pH-neutral substance chitosan-based

The feedstock powder of chitosan dissolved in 2% acetic or hydrochloric acid to obtain a 2% solution of chitosan, which is filtered through fabric filters. Then, the solution of chitosan is alkalinized to pH 7.5 to 8.0 by adding 20-40% of potassium hydroxide or sodium with constant stirring. In the resulting reaction mixture with constant stirring for 5-7 min injected dropwise dichlorohydrin succinic acid in a quantity of 0.1% by weight of the reaction mixture. The ratio of dichlorohydrin succinic acid to the dry weight of chitosan SOS is 70-90oC (to speed up the ripening process) within 1-2 hours the product is squeezed and twice washed with double distilled water to remove salts and reaction products with the subsequent packing and autoclave under a pressure of 0.5 ATM for 30-40 minutes the Finished product has a pH-neutral reaction (pH of 6.0-7.0) and contains 5-20% chitosan and 80-95% water. Specified product may be subjected to freeze drying to a residual moisture content of 2-5 wt. % for long-term storage or use in a dry form.

Examples 2-5. Technology of production of pH-neutral substance on the basis of chitosan with other alleluya agents and other weight ratios with chitosan (examples 2-5) similar to the technique described in example 1. Indicators of technological process of obtaining pH-neutral substance using different alleluya agents (examples 1-5) are given in table.1.

The final product of examples 1-5 is the water content in the structure of chitosan, i.e., has a different degree of viscosity.

Example 6. The technology of obtaining a gel-like substance with the use of organic acids

To produce 1 kg of gel product take 200 g of pH-neutral is Oh acid (final concentration 0.2 wt. %) followed by homogenization to obtain a gel-like final product, which has a pH of 5.5.

Examples 7-14. The technology of obtaining a gel-like substance on the basis of chitosan with other organic acids and pH-neutral substance obtained in accordance with examples 2 through 5, similar to the technique shown in example 6. Indicators of technological process of obtaining a gel-like substance using different pH-neutral substances, prepared in accordance with examples 1-5 are given in table. 2.

Example 15. The technology of obtaining a gel-like substance with the use of the products of microbiological synthesis of

To produce 1 kg of gel product take 150 g pH-neutral product obtained in example 1, and mixed with 850 ml of biomass lactic acid bacteria, Bifidobacterium bifidum strain N 1 with title 109cells/ml and acidity 95oT followed by homogenization of these components to obtain a gel-like end product with a pH of 4.5-5.0.

Examples 16-19. The technology of obtaining a gel-like substance on the basis of chitosan with other products of microbiological synthesis and pH-neutral substance obtained is ocess obtain a gel-like substance using different pH-neutral substances, prepared in accordance with examples 1-5 are shown in table. 3.

Example 20. To prepare diet food product, pH-neutral autoclaved substance prepared in accordance with examples 1-5, mixed with plant extracts and/or fruit syrups, and/or bee products the next time quantitative ratio of components, wt.%:

Plant extracts and/or fruit syrups, and/or bee products - 1,0-10,0

pH-Neutral substance - Rest

Example 21. To obtain immunostimulating and regulating the acidity of the stomach food tools use pH-neutral substance in a dry form or mixed with other dry food additives such as carboxymethylcellulose (CMC) in any proportion.

Example 22. To receive treatment-and-prophylactic food product chitosan-based gel-like substance obtained according to example 10, is mixed with Vinylinum in the ratio of 1:1-10:1.

Example 23. To obtain diet food product chitosan-based gel-like substance obtained according to example 15 are mixed with fruit syrup in a ratio of 10:1.

Example 24. To get to the're asked with resorcinol pharmacological, the Vinylinum, ethyl alcohol, lavender oil (perfume) in the following quantitative ratio of components, wt.%:

Resorcinol pharmacological - 3,0-5,0

Vinylinum - 1,0-2,0

Ethyl alcohol - 10,0-20,0

Lavender - 0,01-0,05

The gel-like substance on the basis of chitosan - Rest

The resulting tool has a disinfectant, exfoliating, whitening, anti-inflammatory effect and can be used in the treatment of acne and dermatitis, as well as against oily skin and hair loss.

Example 25. To receive externally-warming and distracting funds chitosan-based gel-like substance obtained according to example 7 are mixed with tincture of capsicum and Vinylinum, the next time quantitative ratio of components, wt.%:

Tincture of capsicum - 10,0-30,0

Vinylinum - 1,0-3,0

The gel-like substance on the basis of chitosan - Rest

The resulting tool can be used as an external warming remedy for colds, as a distraction for muscle and joint pain of different origin.

Example 26. To obtain cosmetics chitosan-based gel-like substance, the floor is or vitamin E oil the sage oil and preservative, the following quantitative ratio of components, wt.%:

Cocoa butter - 1,0-5,0

Olive oil - 2,0-8,0

Castor oil - 1,0-3,0

Tincture of calendula - 3,0-5,0

10% solution of vitamin E in the oil - 1,0-2,0

Sage oil - 0,01-0,1

Preservative - 0,1-0,5

The gel-like substance on the basis of chitosan - Rest

The resulting cream can be used as a tool for daily skin care and has emollient, nourishing, protective effect.

Example 27. To obtain cosmetics chitosan-based gel-like substance obtained in example 18, is mixed with zinc chloride, magnesium sulfate, selenological sodium, Vinylinum, mint oil (flavoring and preservative, wt.%:

Zinc chloride - 0.02

Sulphate of magnesium, 0.1 to

Selenological sodium - 0,01

Vinylinum - 2,0

Peppermint oil - 0,01

Preservative - 0,25

The gel-like substance on the basis of chitosan - Rest

The resulting tool can be used as a mask to nourish the skin, bleaching age spots and freckles, as well as to stimulate the regeneration of skin cells.

Example 28. To obtain Cosme is ru 14, mixed with glycerol calcium fluoride sodium, oil of the Australian tea tree (flavoring and preservative in the following quantitative ratio of components, wt.%:

Glycyrrhizinate calcium - 0,1-1,0

Sodium fluoride - 0,01-1,0

The oil of the Australian tea tree - 0,01

Preservative - 0,25

The gel-like substance on the basis of chitosan - Rest

Received toothpaste has a disinfectant, refreshing, whitening, anti-inflammatory and action of anti-caries effect.

A long and comprehensive study on the bioactive properties of chitosan make it possible to recommend products made by the proposed method, as immunostimulatory drugs, for example, when used as an adjuvant for immunostimulatory funds with the aim of increasing the production of antibodies by the body. With the introduction of the proposed product with food in the body's immune system and accelerates the development of Lactobacillus bifidus in the digestive system and also ensures that the regulation of the acidity of the stomach (ulcers prevention), which is associated with the ability of chitosan to neutralize the free acid of the stomach to form a protective layer on the walls and hearth is the amount of biologically active additives in toothpaste provides an anti-inflammatory and carisoprodolonline action.

The introduction of a gel-like substance on the basis of chitosan in medical and cosmetic products provides repair and gerontologically properties of the obtained means.

Industrial applicability

The invention can be used in food industry, medicine, cosmetics, veterinary and biotechnology.

1. A method of obtaining a substance based on chitosan for food and pharmaceutical industry, including the preparation of a solution of chitosan in dilute hydrochloric or acetic acid, removing nerastvorim particles of chitosan by filtration or sedimentation and carrying out modifications of chitosan allermuir agent under alkaline conditions at pH 7.0 and 9.0 with the subsequent laundering of the obtained pH-neutral substance, characterized in that as Alliluyeva agent use dichlorohydrin dicarboxylic acid, the reaction is carried out at a temperature of 18 - 25C until the formation of gel-like product structure in a weight ratio of dichlorohydrin dicarboxylic acid and chitosan in terms of dry weight of 1 : 5 - 1 : 25, and the resulting pH-neutral substance chitosan-based autoclave, or dried by lyophilization, or it is injected organic acids, teachings ready gel-like substance with a pH of not more than 6.0.

2. The method according to p. 1, characterized in that as dichlorohydrin dicarboxylic acid used dichlorohydrin succinic acid, or dichlorohydrin glutaric acid, or dichlorohydrin adipic acid, or dichlorohydrin fumaric acid.

3. The method according to p. 1, characterized in that the organic acids used formic, or acetic acid, or benzoic acid, or salicylic acid, or aspirin, or glycol, or nicotine, or deoxybenzoin, or lactic acid in an amount of 0.1 to 5.0% relative to the total weight of the final product.

4. The method according to p. 1, characterized in that as products of microbiological synthesis, containing organic acids using biomass lactic acid bacteria, Bifidobacterium bifidum or Bifidobacterium longum or Lactobacillus acidophilus or serum obtained from biomass of these bacteria, or Baker's yeast autolysate in the amount of 25 - 85% relative to the total weight of the final product.

 

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