RU2346442C1 - Chitosan-containing hydrogel production method - Google Patents

Abstract

FIELD: food products.

SUBSTANCE: method proposed envisages blend of two solutions and the resultant compound degasation and polymerisation. The first solution production process envisages addition of water and ethylenediamine - N,N,N',N' - tetraacetic acid to chitosan or derivatives thereof, mechanical agitation of the resultant compound, further load of acid for pH to be 4.0, heating to produce a solution, load of alkali for deposition of a sediment, the sediment collection and distilled water flushing for pH to be 6.2, further successive load of acid for the sediment complete dissolution, alkali for pH to be 6.2 and acide for pH to be 5.6, centrifugation, distilled water addition and vacuum degasation of the solution thus produced. The second splution is produced by way of having distilled water, acid and sodium or potassium persulphate to N,N,N',N' - tetramethylethylenediamine.

EFFECT: combination of hydrogel plasticity properties with prophylactic and protective properties of chitosan or derivatives thereof to have been preserved after polymerisation.

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Description

The invention relates to the food industry and can be used for the production of chitosan-containing casings for sausage, confectionery and other products.

Artificial casings successfully replace scarce natural raw materials; they are obtained mainly by processing kallogen-containing waste.

A known method of manufacturing a shell by preparing a homogeneous suspension. The method is used in the domestic meat industry. According to organoleptic, physico-mechanical and physico-chemical parameters, the shell must meet the requirements and standards of TU 9219-094-00008064-96 "Protein artificial shell" Belkozin ". In the method of producing the shell (Technical instruction" Belkozin "OTI 1,0-4, 2) a hydrolyzate-chitosan-pigment (GHP) suspension is prepared, for which, based on the dry matter of collagen material, a hydrolyzate of about 1.6%, chitosan about 0.15%, a pigment about 2% are taken. protein hydrolyzate solution, 4% chitosan acetic acid solution and pigment paste, for example a universal masterbatch pigment (UPC - CM 704).

The disadvantage of this method is that the resulting shells do not have sufficient plastic properties.

There is also known a method of producing a gel based on chitosan, which includes preparing a solution of chitosan in dilute acid, mixing the resulting solution with a hydrophobic substance, mixing the mixture to obtain an emulsion, conducting a covalent fixation of chitosan in the composition of the emulsion by introducing a bifunctional reagent capable of forming transverse covalent crosslinking between chitosan molecules, followed by washing and filtering the resulting product (ed. certificate of the USSR N 827492, 05/07/1981). The product of this technology is a cross-linked gel based on chitosan, which is a rigid microspherical granule.

The disadvantages of this technical solution is that the hard microgranular gels based on chitosan obtained by this method are not suitable components for food products, because do not have sufficient plastic properties and are not absorbed by the body.

In addition, the known methods do not provide for the most complete use of the characteristics of chitosan and its derivatives, corresponding to their biological and preventive properties.

The objective of the present invention is to obtain a quality product with high organoleptic and prophylactic indicators.

The problem is solved due to the fact that according to the claimed method for producing a chitosan-containing hydrogel, two solutions are mixed, while distilled water and ethylenediamine-N, N, N ′, N′-tetraacetic acid (EDTA) are added to the chitosan or its derivatives. stirring is carried out, after which acid is added to pH 4.0 and heated to dissolve, then alkali is added until a precipitate is formed, which is separated and washed with distilled water to pH 6.2, acid is added until it is dissolved, and then alkali to a pH of 6.2, then acid is introduced to a pH of 5.6, after which centrifugation, addition of distilled water and degassing of the obtained first solution are carried out under vacuum, and to obtain a second solution to N, N, N ′, N′-tetramethylethylenediamine ( TEMED) add distilled water, acid or sodium or potassium persulfate. After mixing the two solutions, the resulting mixture is degassed and polymerized.

Thus, according to the above method, the final product is obtained - a chitosan-containing hydrogel.

The hydrogel obtained by the claimed method can be used as shells for sausage, confectionery and other products, as well as for medical and cosmetic purposes in cases where it is necessary to create a protective shell on the skin surface.

The technical result according to this invention is to provide the possibility of manufacturing a high quality product that provides a shell with highly plastic properties, as well as maintaining the preventive and protective properties of chitosan and its derivatives in a polymerized state.

Tests were carried out, as a result of which it was found that the shell-forming substance of the proposed composition has increased stretching and strength, which, when heat treated, allows it to stretch 6 times without breaking the shell, and when cooled, it forms an elastic film that has a tensile strength of 1 kg / cm, which allows you to keep the desired shape of the product, chitosan prevents the development of microorganisms on the surface of the product, thereby increasing the shelf life of the product; the resulting film has a sealed property that does not allow microorganisms to penetrate the main product, this film allows you to maintain the humidity regime required for the finished product.

The method for producing chitosan-containing hydrogel according to the invention is illustrated by the following examples, which, however, do not cover, and even more so do not limit the entire scope of the claims of this invention.

Example 1

Prepare the first solution as follows. To 44 g of chitosan add 500 ml of distilled water and 2.5 ml of ethylenediamine-N, N, N ′, N′-tetraacetic acid (EDTA) and stirring is carried out. Next, hydrochloric acid (HCl) is introduced to a pH of 4.0 and heated to dissolve. Potassium hydroxide (KOH) (alkali) is added until a precipitate forms. The resulting suspension is poured onto a sieve, the precipitate on the sieve is washed with distilled water to a pH of 6.2. About 25 ml of acetic acid is added until the precipitate is dissolved, and then KOH (alkali) is added to a pH of 6.2. Acetic acid is then added to a pH of 5.6 and centrifuged to separate solids. After centrifugation, distilled water is added to a total volume of 500 ml. The resulting solution was degassed under vacuum.

To obtain a second solution, 75 μl of N, N, N ′, N′-tetramethylethylenediamine (TEMED) are taken, 2 ml of distilled water, 75 μl of glacial acetic acid and 20 mg of sodium persulfate are added. The second solution is mixed with 0.04 ml of the first solution, after which the resulting mixture is degassed and polymerized, resulting in a chitosan-containing hydrogel.

Example 2

Prepare the first solution as follows. To 44 g of chitosan succinic acid, add 500 ml of distilled water and 2.5 ml of ethylenediamine-N, N, N ′, N′-tetraacetic acid (EDTA) and stirring. Then ascorbic acid is introduced to a pH of 4.0 and heated to dissolve. Sodium hydroxide (NaOH) (alkali) is added until a precipitate forms. The suspension is poured onto a sieve, the precipitate on the sieve is washed with distilled water to a pH of 6.2. Ascorbic acid is added until the precipitate is dissolved, and then NaOH (alkali) is added to a pH of 6.2. Then ascorbic acid is introduced to a pH of 5.6 and centrifuged to separate solids. After centrifugation, distilled water is added to a total volume of 500 ml. The resulting solution was degassed under vacuum.

To obtain a second solution, 75 μl of N, N, N ′, N′-tetramethylethylenediamine (TEMED) are taken, 2 ml of distilled water, 75 μl of acid and 20 mg of potassium persulfate are added. The second solution is mixed with 20 ml of the first solution, after which the resulting mixture is degassed and polymerized, resulting in a chitosan-containing hydrogel.

Claims (1)

A method of producing a chitosan-containing hydrogel, characterized in that it involves mixing two solutions, degassing the mixture and polymerizing it, while distilled water and ethylenediamine-N, N, N ′, N′-tetraacetic acid are added to the chitosan or its derivatives stirring is carried out, after which acid is added to pH 4.0 and heated to dissolve, then alkali is added until a precipitate is formed, which is separated and washed with distilled water to pH 6.2, acid is added until it is dissolved, and then alkali to pH 6.2, then acid is introduced to pH 5.6, then centrifuged, distilled water is added and the first solution is degassed under vacuum, and to obtain a second solution to N, N, N ′, N′- distilled water, acid and sodium or potassium persulfate are added to tetramethylethylenediamine.