LV10367B - Process for producing gelatin - Google Patents

Abstract

The innovation relates to the technology of gelatin production from soft raw material containing collagen, for example hides, and can be used in the production of victual gelatin. Hides after shredding are processed for 14 - 18 hours with ferment preparation mixture of proteosubtilin U3X and multienzyme MEK (proportion 1:3-5) at the temperature of 12 - 20 degrees C at pH 8.0 - 10.5. The ferment mixture is added to 0.1 - 0.2 percent of raw material mass. Outcome of gelatin is 16.4 - 17.2 percent, dynamic viscosity till 45.5 mPa/s, 5 percent of clarity of gelatin solution above 70 %.

Description

LV 10367

METHOD OF GELATIN ACQUISITION

The patented technique refers to the technology of obtaining gelatine from a raw collagen-containing raw material, is made from "bovine skins" and can be used for the production of food gelatine.

The scientific and patent literature describes methods for obtaining gelatine using various acids, flanks, salts, or combinations thereof (1, 2, 3) as well as enzyme preparations (4, 5, 6) for processing raw materials, as described in the VFR patent (4). the method by which the raw material of bovine foot joints is treated with a proteolytic enzyme to which urea has been added.

In contact with the technology described in the USSR authorship certificate (5), the raw collagen-containing raw materials (pigs or cattle skins) are ground, defrosted, 3 hours. o Wash with water to pH 8.0, heat up to 38 C and liquid at 2 3 h. treated with enzyme - proteosubtilin x 10x or protorizine Γ 10x_ Enzyme content 0.1% by weight of the starting material. Then, the enzyme solution is decanted, 2 st. little # with running water. Next is 3-6 hrs. long treatment with saline at room temperature and pH 2-3. After treatment with brine-2-bi raw material, wash with water until pH 5.0 and 5-6 are extracted by collagen at 55-60 ° C and fluid ratio of 2-3, gelatine yields up to 16.4%. 5 quantities of raw materials.

The disadvantages of the known method, despite the relatively high yield of gelatin, are as follows: decrease in the quality of gelatin due to partial collagen degradation to the peptides, because the treatment with the enzyme takes place at a relatively high temperature of 38 ° C, which in turn makes the process itself more complicated - necessary provide the required temperature modes. Due to the use of purified proteolytic enzymes with their specific activity spectrum, the cost of gelatin 15 is higher - the resulting product has increased color because no mucopolysaccharide is separated. The method of obtaining gelatin described in the USSR autorapl (6) has been selected as the prototype of the invention. 20 According to the prototype gelatin is obtained as follows: 2 t of bovine collagen-containing raw material is chopped into pieces of 50-100 mm, 6 h. wash with running water to a peak of 8.5. After washing, pour warm water (36-40 C), liquid ratio 1.5. Add 20 kg of sodium carbonate (Na 00) to degrease the raw material. 2 3 25 - 3 - - 3 -LV 10367 After 3 hours of degreased starting material. treated with

alkaline protease - proteosubli Q 1x at pH 9.0-10.5 and temperature 36-40 C. Amount of enzyme added - 0.02-0.05% by weight of starting material. After treatment with enzyme raw material 2 h. wash with running water, tel. neutralize with hydrochloric acid at pH 3.5 and wash to pH 5.5.

The prepared raw material is loaded into the boiling pot, allowing to drain the excess water, pouring drinking water and boiling broths. Broth boiling temperatures are as follows; o

First broth - 45 - 55 C o

Second broth - 55-60 ° C

Third broth - 60 - 65 ° C

Fourth Broth - 65 - 70 C Control cooking time and broth concentration. All further operations for gelatin are made by known technology.

The selected prototype has the following disadvantages: the complexity of the technological process and the loss of collagen during the processing of the raw material at a temperature of 36-40 C, which also contributes to the decrease of the quality of the gelatin (lower viscosity, higher end color). Using the purified enzyme preparation proteosubtilin Γ 10x in the production process increases the cost of gelatin - 4.

The patented method achieves these shortcomings by simplifying the technological process and maintaining the high yield and quality of gelatin 5.

In contact with a patentable invention, gelatin is obtained from bovine animals < & treated with the enzyme preparation proteosubtilin x 3x and o multienzyme MEK at a temperature of 12-20 C and 10 pH 8.0-10.5, where the weight ratio of the enzyme preparations proteosubtilin Γ 3x and mnti-enzyme MEK in the mixture is 1; 3-5 and added 0.1-0.2% by weight of the starting material.

The patentable invention provides the following positive effect: using an enzyme bag at a concentration of 0.1-0.2% of the weight of the starting material at temperatures of 12-20 C, which are lower than the optimum temperature required for enzyme activity, the structure of the polypeptide chains in the collagen is preserved to the maximum. it is not split up into peptides. As it is known to obtain good quality gelatin, the following prerequisites are needed: the weakening of the bonds held by the polypeptide chains in the collagen structure without the simultaneous cleavage of the peptide bonds in the chains itself, a soft extraction process with a pH close to the LV 10367-5 collagen isoelectric point, in the process of gelatin production, the three-dimensional (spatial) structure of collagen due to the disruption of hydrogen bonds is transformed into 5 two-dimensional (plane) structures; wherein the polypeptide chains remain linked to each other by means of the salt bridges *. Shrinking the salt bridges * in such a two-dimensional structure, while not breaking the peptide bonds in the major chains, allows for the formation of particles consisting of 5-6 covalently linked polypeptide chains. Such a collagen three-dimensional structure breakdown product containing as many large polypeptide fragments has the ideal clotting ability. Thanks to a patentable technological process, these 15 conditions are maximized. A mixture of enzymes that simultaneously possess proteolytic, amylolytic, β-glucanase, lysozyme u, c not only release collagen from ballast proteins, but also digest mucopolysaccharides and destroy harmful microflora, thereby reducing gelatin color and the amount of microorganism in it.

Due to the use of technical untreated enzyme preparations in the technological process, the cost of the final products is reduced. - 6 - Thus, thanks to the patentable method is. high-quality gelatin with high dynamic viscosity - over 30 mPa / sec, better clot formation and low. color (clarity of 5% gelatin solution above 70%).

The following examples illustrate the invention: 1. dairy. 200 g of cattle skin is crushed to 50-100 mm, washed twice with cold water, then poured so much water into the flask to cover the skin and add 0.05 g of proteosubtilin x 3x and 0.15 g of multienzyme ināti, previously dissolved in a small amount. amount of water. Mixture o 14 h. at 12 C and pH 8.0, then the enzyme solution is discarded and the starting material is 24 h. soak with cold water; then pour fresh water and acidify to ρΉ 2.5 with 5% hydrochloric acid solution and pass to 6 h with running water to pH 5.0. The raw material is placed in a beaker o and broth 9 is boiled for 9 h. at 65-75 ° C, 19.2 g is obtained

gelatin with dynamic viscosity f \ _ - 40.5 mPa / sec. II o broth boil 5.5 st. at 85-90 ° C, 13.6 g of gelatin are digested with λ - 19.5 mPa / sec. Total gelatin yield - 16.4%. Example 2: - 7 - - 7 -LV 10367

Beef skins are prepared in the same way as in l. 0.06 g of proteosubtilin is added. X 3x and 0.24 g of MTI, previously dissolved in a small amount of water. Mixtures o 16 h. withstand 15 C and pH 9.5, further technological operations are performed similarly to Example 1. The 8o I broth produces 19.5 g of gelatin with a flab of 45.5 mPa / sec. 14.9 g of gelatin with 21.7 mPa / sec are obtained from broth II. Total gelatin yield - 17.2%. Example 3:

Bovine skins are prepared analogously to example 1. 0.08 g of proteosubtilin Γ 3x and 0.32 g of multienzyme MEK, previously dissolved in a small amount of water, are added. o

Mixtures 18 h. resistant to 20 C and pH 10,5. Next, the technological operations are performed analogously to example 1. \ t

From broth I, 18.2 g of gelatin is obtained with q__- 41.7 stPa / sec. From broth II, 15.4 g of gelatine is obtained with an oil of 19.3 m Pa / sec. Total gelatin yield 16.8%.

The patentable invention enables high-quality gelatin to be obtained (dynamic viscosity up to 45.5 mPa / sec, 5% gelatin solution clarity above 70%), while ensuring its high yield (16.4-17.2%) and lowering the cost price.

The selected process parameters are the optimally patentable method. By reducing or increasing the pH, - 8 - temperature, the weight ratio of the enzyme preparations to be added and the weight, it is not possible to obtain gelatin with the above mentioned quality parameters and find out. 5

LIST OF LITERATURE 1. HnKpKtKOBa Γ.Α., ABTope * fepaT Ha ccascKarae vhekoA CTe-neHM Kauzsnsara TexHtnecioix nayx " SccjjBjvmssHiee h

10 pačoTKa cnocoča npoM3BQzjcTBa atenarisHa juih nemouuHcscisK uB & yocx, 1981. 2. Οοκολοβ A.A_ ίλ Λρ. 660-713. 15 3. TeKHonorMHecKaH MHCTpyxmuī from npcaasBoacTBV menamaHa ot 26.06.89 r., HocKBa, 1990 4. VER patent No. 2813075, SIC C08 L 89/06, 1979. 5. USSR authorship certificate No. 1126586, SIC 009 H 1/00, 1984 6th USSR authorship order No. 851809, SIC A 23 J 1/10, 1980.

Claims (3)

PATENT FORMULA GELATINE PREPARATION METHOD BASED ON SOFT COLLECTION OF COLLAGENATED RAW MATERIALS SUCH AS BEEF SKINS, TREATED WITH ENZYME PREPARATION AND HYDROCHLORIC WATER, WASHED WITH WATER AFTER PRE-TREATMENT WITH ENZYME AND HYDROCHLORIC ACID, AND EXCESSED GELATINE AT that soft collagen-containing starting material after 10 shredding for 14-18 hours. treated with an enzyme preparation of a mixture of proteasubtilin χ3χ and a multienzyme MES at o 12-20 C and a pH of 8.0-10.5, wherein the weight ratio of the enzyme preparations proteosubtilin to multienzyme MEK is 1: 3-5 and added to 0.1 -0.2 X by weight of 15 inputs. The patented process relates to a technology for obtaining gelatin from a soft collagen-containing raw material, such as bovine hides, and is useful for the production of edible gelatin. The scientific and patent literature describes methods for obtaining gelatin using various acids, alkalis, salts or combinations thereof (1, 2, 3) as well as enzyme preparations (4, 5, 6). The German patent (4) describes a method according to which raw material of bovine leg joints is treated with a urea-containing proteolytic enzyme. According to the USSR Author (5), the description of their technology, soft collagen-containing raw material (pig or bovine hides), grind, degrease, 3 hours. o Wash with water to pH 8.0, then warm to 38 ° C and at a liquid ratio of 2 3 h. treated with the enzyme proteosubtilin Γ 10x or prothorizine. Γ 10x_ Quantity of enzyme 0,1 * by weight of starting material. The enzyme solution is then discarded and the raw material is stirred for 2 hours. wash with running water. Next, 3-6 hours. long treatment with hydrochloric acid at room temperature and pH 2-3. After treatment with saline, wash the raw material with water until pH 5.0 and 5-6 h. o Extract collagen at 55-60 C and a liquid ratio of 2-3, yielding up to 16.4% gelatin based on the raw material hardness. partial collagen degradation to peptides, as the enzyme treatment takes place at a relatively high temperature of 38 ° C, which in turn complicates the technological process itself. Due to the use of purified proteolytic enzymes with their specific activity spectrum in the process, the cost price of gelatin 15 is higher - the resulting product has a higher coloration because no mucopolysaccharides are separated. The method of obtaining gelatin described in the USSR Authorization (6) has been chosen as the prototype of the invention. 20 According to the prototype, gelatin is obtained as follows: Example 1: Grind 200 g of beef skin to 50-100 mm, wash twice with cold water, then add enough water to cover the skin and add 0.05 g of proteosubtilin Γ 3x and 0.15 g of multienzyme MEK previously dissolved in a small of water. Mixture o 14 hours holds at 12 C and pd 8.0, then drains the enzyme solution and feeds for 24 hours. soaked in cold water; then pour in fresh water and acidify to 2.5 with 5% hydrochloric acid solution and hold for 6 hours, wash with running water to pH 5.0. Place the stock in a beaker and boil the broth for 9 hours. at 65-75 ° C, 19.2 g of gelatin with a dynamic viscosity Q_-40.5 mPa / sec are obtained. II o broth cook 5,5 hours. at 85-90 ° C, 13.6 g of gelatin are obtained with a? - 19.5 mPa / sec. The overall yield of gelatin is 16.4%. Example 2: - 7 Bovine hides are prepared in the same way as 1, Add 0.06 g of proteosubtilin. Γ 3s. and 0.24 g / ml of mictusimek, previously dissolved in a small amount of water. Kaisijuma o 16 hours withstands at 15 C and pH 9.5. The lower 3 technological operations are performed analogously to Example 1®. So I broth yields 19.5 g of gelatin with Π. - 45.5 mPa / sec. So II broth yields 14.9 g of gelatin with ίη_ - 21.7 mPa / sec. Total gelatine yielded - 17.2%. 2 3 - 3 After 3 hours of fat-free raw material. treated with alkaline protease - proteosubtilin Γ 10x at pH o 9.0-10.5 and temperature of 36-40 C- 0.02-0.05% by weight of the added enzyme. After treatment with the enzyme starting material, it is washed with running water for 2 hours, neutralized with acidic acid at pH 3.5 and washed to pH 5.5 for 2 hours. The prepared raw material is loaded into the boiler, allowed to drain excess water, poured drinking water and boiled broths. Broth cooking temperatures are as follows: o First broth 45-55 ° C Λ Second broth O 55-60 ° C Third broth o 60-65 ° C Fourth broth o 65-70 ° C Cooking duration and broth concentration All subsequent operations for the production of gelatine are carried out by known technology. The following disadvantages are sent to the chosen prototype: the complexity of the technological process and the loss of collagen during the processing of the starting material at a temperature of 36-40 ° C, which also contributes to the lowering of the gelatin quality (lower viscosity, higher color of the finished product). Gelatin is increased by the use of proteosubtilin Γ 10x purified in the manufacturing process - 4 self-stamping. The patented method eliminates these disadvantages by simplifying the technological process and maintaining high levels of gelatin 5 Output and Quality. In combination with the patented inventive gelatin, is obtained from bovine skin®, which has a shredding effect of 14-18 hours. treated with enzyme preparation Proteosubtilin na Γ 3.x and o Mnl enzyme MEK bags at 12-20 C and 10 pH 8.0-10.5, wherein the enzyme preparations are proteosubtilin The mass ratio of x3x and mnl-thymyme MEK in the mixture is 1: 3-5 and add 0.1-0.2% by weight of the starting material. The patentable invention provides the following positive effect: by using an enzyme mixture At a concentration of 0.1-0.2% by weight of the starting material at a temperature of 12-20 C below the optimum temperature required for enzyme activity, the structure of the polypeptide chains in collagen is maximally preserved, without being cleaved to the peptides. 20 The following prerequisites for obtaining good quality gelatin are: weakening of the bonds that hold the polypeptide chain in the collagen structure without simultaneously breaking the peptide bonds within the chain itself, a soft extraction process with a near pH - 5 for the isoelectric point of collagen, the three-dimensional (three-dimensional) structure of collagen undergoes hydrogen bonding during the gelatin production process 5 in a two - dimensional (plane) structure,. wherein the polypeptide chains remain attached to one another by salt bridges. Shrinking of salt bridges in such a two-dimensional structure without simultaneously breaking the peptide bonds in the backbone allows the formation of particles which 10 consists of 5-6 covalently linked polypeptide chains. Such a three-dimensional collagen product of collagen, which contains as many large polypeptide fragments as possible, has ideal clot-forming capabilities. Thanks to a patentable technological process: 15 conditions are maximized. Mixture of enzymes having at the same time proteolytic, amylolytic, β - glucanase, lysozyme, etc. not only release collagen from ballast proteins, but also decompose mucopolysaccharides and destroy harmful microflora, 20 thus reducing the color and the amount of microorganisms in the gelatin. The use of technical crude enzyme preparations in the technological process reduces the cost price of the final products. - 6 Thus, the patented process produces high-quality gelatin with a high dynamic viscosity of over 30 mPa / sec, superior "clot-forming ability" and low color (5% gelatin solution clarity over 70%). The invention is illustrated by the following examples; Grind 2 tonnes of bovine collagen feedstock into 50-100 mm pieces for 6 hours. wash with running water until drip 8.5. After washing, pour warm water (36-40 C), liquid ratio 1.5. To the raw material 25 g of fat, add 20 kg of sodium carbonate (Na 00). Example 3. The bovine skins are prepared analogously to Example 1. Add 0.08 g proteosubtilin Γ 3x and 0.32 g multienzyme MEK previously dissolved in a small amount of water », o The mixture was stirred for 18 h. withstands at 20 C and pH 10.5. Next, the technological operations are performed analogously to Example 1. From broth I pour 18.2 g of gelatin with q __- 41.7 mPa / sec. So II broth infuses 15.4 g of gelatin with 19.3 m Pa / sec Total gelatin yields 16.8%. The patented invention provides high quality gelatin (dynamic viscosity up to 45.5 mPa / sec, 5% gelatin solution clarity above 70%) while providing high yield (16.4-17.2%) and lower cost. The selected process parameters are optimal for the patentable method. By lowering or increasing pH, temperature, weight ratios and weight of enzyme preparations added, it is not possible to obtain gelatin with the above quality characteristics and yield.