CN113896785B - Preparation method of anti-crosslinking gelatin - Google Patents
Preparation method of anti-crosslinking gelatin Download PDFInfo
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- CN113896785B CN113896785B CN202111076057.6A CN202111076057A CN113896785B CN 113896785 B CN113896785 B CN 113896785B CN 202111076057 A CN202111076057 A CN 202111076057A CN 113896785 B CN113896785 B CN 113896785B
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- 108010010803 Gelatin Proteins 0.000 title claims abstract description 74
- 229920000159 gelatin Polymers 0.000 title claims abstract description 74
- 239000008273 gelatin Substances 0.000 title claims abstract description 74
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 74
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 74
- 238000004132 cross linking Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000003292 glue Substances 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 14
- 238000013329 compounding Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 230000001954 sterilising effect Effects 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 7
- 238000013467 fragmentation Methods 0.000 claims abstract description 7
- 238000006062 fragmentation reaction Methods 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 35
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 8
- 239000003456 ion exchange resin Substances 0.000 claims description 7
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- 239000003957 anion exchange resin Substances 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002775 capsule Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 125000003172 aldehyde group Chemical group 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000003729 cation exchange resin Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 239000007901 soft capsule Substances 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000004475 Arginine Substances 0.000 description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 2
- 239000004472 Lysine Substances 0.000 description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007854 aminals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229940124531 pharmaceutical excipient Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229940126589 solid medicine Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011686 zinc sulphate Substances 0.000 description 1
- 235000009529 zinc sulphate Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
- A61K9/4825—Proteins, e.g. gelatin
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Biochemistry (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Zoology (AREA)
- Gastroenterology & Hepatology (AREA)
- Animal Behavior & Ethology (AREA)
- Biophysics (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Pharmacology & Pharmacy (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a preparation method of anti-crosslinking gelatin, which comprises the following steps: s1, selecting a gelatin extraction raw material, carrying out fragmentation treatment, and washing; s2, soaking the raw materials in acid liquor with the pH value of 0.8-3 or alkali liquor with the pH value of 11-13; s3, cleaning the raw materials by using water, acid liquor or alkali liquor respectively in sequence and neutralizing until the pH value is 6.5-8.0; s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times; s5, adding acid liquor or alkali liquor into the gelatin solution in the concentration of 40-60% S4 to control the pH value to be 1-3 or 11-13 for soaking, neutralizing and washing, filtering small molecular gelatin with the pH value below 20000Da by an ultrafiltration membrane, and measuring the solid content; s6, compounding the gelatin solutions in the S4 and the S5 according to the proportion of 1-3:7-9 of the fixed object; s7, ion exchange is carried out on the concentrated gelatin solution; s8, concentrating again, drying, sterilizing and crushing to obtain the anti-crosslinking gelatin, which has the advantage of good anti-crosslinking property.
Description
Technical Field
The invention relates to the technical field of pharmaceutical excipients, in particular to a preparation method of anti-crosslinking gelatin.
Background
The soft capsule is a capsule prepared by processing and sealing liquid medicine or solid medicine in soft capsule wall material. The soft capsule wall material is prepared by mixing gelatin, glycerol or other proper medicinal auxiliary materials. The soft capsule prepared from conventional gelatin has the problem of easily cross-linking capsule shells during the later storage and transportation processes due to the chemical properties of the external environment and the content (most of traditional Chinese medicine extracts), and forms a water-insoluble film to delay or prevent the release of the capsule content.
The reaction mechanism of the capsule shell for crosslinking is mainly divided into two parts, namely, the gelatin itself undergoes crosslinking reaction under the influence of storage environment, side chain amino groups of lysine and arginine in the gelatin are oxidized into aldehyde groups, and the aldehyde groups and the amino groups undergo further aminal reaction to generate crosslinking. Secondly, the content of the capsule contains aldehyde groups, and the aldehyde groups directly react with side chain amino groups of lysine and arginine to generate crosslinking.
Therefore, the development of gelatin with an anti-crosslinking effect has positive significance for the development of the pharmaceutical industry.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of anti-crosslinking gelatin, and the prepared gelatin has an anti-crosslinking effect.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing an anti-crosslinking gelatin, comprising the steps of:
s1, raw material pretreatment: selecting gelatin extraction raw materials, carrying out fragmentation treatment, and washing;
s2, raw material acid or alkali treatment: soaking the raw materials in acid solution with pH of 0.8-3 or alkali solution with pH of 11-13;
s3, water washing neutralization: sequentially cleaning the raw materials with water, acid solution or alkali solution respectively, and neutralizing to pH 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, gelatin is dissolved and degraded: adding acid liquor or alkali liquor into 40-60% of gelatin solution in S4 to control pH to 1-3 or 11-13 for soaking, neutralizing and washing, filtering with ultrafiltration membrane to obtain small molecular gelatin with molecular gelatin concentration below 20000Da, and determining solid content;
s6, compounding: compounding the gelatin solutions in S4 and S5 according to the proportion of 1-3:7-9 of the fixed object;
s7, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s8, post-processing: concentrating again, drying, sterilizing, and crushing to obtain the crosslinking-resistant gelatin.
Preferably, in S2, the soaking time of the alkali liquor is 2-4 months.
Preferably, in S5, the soaking condition of the acid solution or the alkali solution is that the acid solution or the alkali solution is soaked for 6 to 24 hours at the temperature of 50 to 80 ℃.
Preferably, after concentration of S9, zinc sulphate is added in an amount of 0.2-0.6% by weight of gelatin.
Preferably, the sterilization temperature is 130-150 ℃.
Preferably, the ion exchange employs a series of columns of a strongly acidic ion exchange resin and a strongly basic anion exchange resin.
Preferably, in S2, the raw materials are soaked in an acid solution with the pH value of 0.8-3.
In summary, the invention has the following beneficial effects:
1. filtering gelatin thin liquid obtained by extracting gelatin, filtering macromolecular particles, filtering by ion exchange resin to remove intermediate particle impurities such as salt, metal ions, acid radical ions, chromogen and the like, wherein an ultrafiltration membrane mainly removes intermediate molecular weight organic matters and partial salt and partially retains the intermediate molecular weight organic matters and partial salt, so that the retained part has a certain concentration range, and the applicant discovers through a large number of experiments that the retained matters in the concentration range have a certain anti-crosslinking effect on subsequently prepared capsule products.
2. By the preferred process steps, the concentration factor can be increased, so that the time of the drying process is greatly shortened, and simultaneously, the high viscosity and Gao Kangdong force of the gelatin are ensured.
3. By adding zinc sulfate to the concentrated gelatin and drying the gelatin powder to form zinc sulfate-coated particles, the applicant has found through a number of experiments that the addition of zinc sulfate to gelatin can improve its freezing resistance and crosslinking resistance.
Detailed Description
Examples
Example 1
A method for preparing an anti-crosslinking gelatin comprising the steps of:
s1, raw material pretreatment: selecting pigskin gelatin extraction raw materials, carrying out fragmentation treatment, and washing with water;
s2, raw material acid or alkali treatment: soaking the raw materials in sodium hydroxide aqueous solution with pH of 11-13 or sulfuric acid aqueous solution with pH of 0.8-3 for 2 months;
s3, water washing neutralization: sequentially cleaning the raw materials by using water, sulfuric acid water or sodium hydroxide water solution respectively and neutralizing until the pH value is 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, gelatin is dissolved and degraded: adding 50% of gelatin solution in S4 into the sodium hydroxide solution obtained by separation and recovery in S3, controlling the pH to be 11-13, soaking for 6h at 50-80 ℃, neutralizing and washing with water, filtering small molecular gelatin with the concentration of below 20000Da by an ultrafiltration membrane, and measuring the solid content;
s6, compounding: compounding the gelatin solutions in S4 and S5 according to the proportion of 1:3 of the fixed object;
s7, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s8, post-processing: concentrating again, adding zinc sulfate accounting for 0.2-0.6% of the weight of the concentrated gelatin, drying, sterilizing at 130-150deg.C, and crushing to obtain the final product.
Wherein the ion exchange resin is a serial column of 732 type styrene strong acid cation exchange resin and 717 type styrene strong base anion exchange resin of Laided environmental engineering Co.
Comparative example
Comparative example 1
A method for preparing an anti-crosslinking gelatin comprising the steps of:
s1, raw material pretreatment: selecting pigskin gelatin extraction raw materials, carrying out fragmentation treatment, and washing with water;
s2, raw material alkali treatment: soaking the raw materials in sodium hydroxide aqueous solution with pH of 11-13 for 2 months;
s3, water washing neutralization: respectively cleaning the raw materials by using water and sulfuric acid water solution in sequence and neutralizing until the pH value is 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, gelatin is dissolved and degraded: adding 50% of gelatin solution in S4 into the sodium hydroxide solution obtained by separation and recovery in S3, controlling the pH to be 11-13, soaking for 6h at 50-80 ℃, neutralizing and washing with water, filtering small molecular gelatin with the concentration of below 20000Da by an ultrafiltration membrane, and measuring the solid content;
s6, compounding: compounding the gelatin solutions in S4 and S5 according to the ratio of 1:2 of the fixed object;
s7, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s8, post-processing: concentrating again, adding zinc sulfate accounting for 0.2-0.6% of the weight of the concentrated gelatin, drying, sterilizing at 130-150deg.C, and crushing to obtain the final product.
Wherein the ion exchange resin is a serial column of 732 type styrene strong acid cation exchange resin and 717 type styrene strong base anion exchange resin of Laided environmental engineering Co.
Comparative example 2
A method for preparing an anti-crosslinking gelatin comprising the steps of:
s1, raw material pretreatment: selecting pigskin gelatin extraction raw materials, carrying out fragmentation treatment, and washing with water;
s2, raw material alkali treatment: soaking the raw materials in sodium hydroxide aqueous solution with pH of 11-13 for 2 months;
s3, water washing neutralization: respectively cleaning the raw materials by using water and sulfuric acid water solution in sequence and neutralizing until the pH value is 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s6, post-processing: concentrating again, adding zinc sulfate accounting for 0.2-0.6% of the weight of the concentrated gelatin, drying, sterilizing at 130-150deg.C, and crushing to obtain the final product.
Wherein the ion exchange resin is a serial column of 732 type styrene strong acid cation exchange resin and 717 type styrene strong base anion exchange resin of Laided environmental engineering Co.
Comparative example 3
A method for preparing an anti-crosslinking gelatin comprising the steps of:
s1, raw material pretreatment: selecting pigskin gelatin extraction raw materials, carrying out fragmentation treatment, and washing with water;
s2, raw material alkali treatment: soaking the raw materials in sodium hydroxide aqueous solution with pH of 11-13 for 2 months;
s3, washing and neutralizing the raw materials by water and sulfuric acid aqueous solution respectively in turn, and neutralizing the raw materials until the pH value is 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, gelatin is dissolved and degraded: adding 50% of gelatin solution in S4 into the sodium hydroxide solution obtained by separation and recovery in S3, controlling the pH to be 11-13, soaking for 6h at 50-80 ℃, neutralizing and washing with water, filtering small molecular gelatin with the concentration of below 20000Da by an ultrafiltration membrane, and measuring the solid content;
s6, compounding: compounding the gelatin solutions in S4 and S5 according to the proportion of 1:3 of the fixed object;
s7, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s8, post-processing: concentrating again, sterilizing at 130-150deg.C, drying, and pulverizing to obtain the final product.
Wherein the ion exchange resin is a serial column of 732 type styrene strong acid cation exchange resin and 717 type styrene strong base anion exchange resin of Laided environmental engineering Co.
Performance test
Test of anti-crosslinking Effect: preparing a sample into a gelatin solution with the concentration of 20wt%, carrying out water bath heat preservation at 50 ℃, and dropwise adding a crosslinking inducer: 37% (v/v) formaldehyde, using a rotational viscometer to measure the viscosity change of the solution, recording the time required for the viscosity to reach 3.0 mPa.s, recording the time as 1 in example 1, and calculating the ratio of the time in each example, wherein the larger ratio represents the better crosslinking resistance of the gelatin.
Freezing force test: the samples were prepared as 6.67wt% gelatin solutions and their freezing force was measured with a freezing force tester at 10 ℃.
Table 1, performance test table
| Ratio of time length | Freeze power (Bloom g) | |
| Example 1 | 1 | 309 |
| Comparative example 1 | 0.7 | 289 |
| Comparative example 2 | 0.6 | 286 |
| Comparative example 3 | 0.8 | 264 |
The present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (3)
1. A method for preparing an anti-crosslinking gelatin, comprising the steps of:
s1, raw material pretreatment: selecting gelatin extraction raw materials, carrying out fragmentation treatment, and washing;
s2, raw material alkali treatment: soaking the raw materials in alkali liquor with pH of 11-13 for 2 months;
s3, water washing neutralization: sequentially cleaning the raw materials with water and acid liquor respectively, and neutralizing until the pH value is 6.5-8.0;
s4, extracting glue: adding the raw materials into a glue extraction pot, adding warm water at 50-80 ℃ for immersing, boiling until the concentration of the glue reaches 2-5%, and extracting for 6 times;
s5, gelatin is dissolved and degraded: adding alkaline solution into 40-60% of gelatin solution in S4 to control pH to 11-13, soaking for 6h at 50-80deg.C, neutralizing, washing with water, filtering with ultrafiltration membrane to obtain small molecular gelatin below 20000Da, and determining solid content;
s6, compounding: compounding the gelatin solutions in S4 and S5 according to the proportion of 1:3 of the fixed object;
s7, deionized and purifying: ion-exchanging the concentrated gelatin solution;
s8, post-processing: concentrating again, adding zinc sulfate 0.2-0.6% of gelatin weight, drying, sterilizing, and crushing to obtain crosslinking-resistant gelatin.
2. The method for preparing the crosslinking-resistant gelatin according to claim 1, wherein: the sterilization temperature is 130-150 ℃.
3. The method for preparing the crosslinking-resistant gelatin according to claim 1, wherein: the ion exchange adopts a series column of a strong acid ion exchange resin and a strong alkaline anion exchange resin.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB568182A (en) * | 1943-04-21 | 1945-03-22 | Andrew Vigodny | Improvements relating to the treatment of skin and leather materials |
| GB628757A (en) * | 1945-11-27 | 1949-09-05 | Kodak Ltd | Improvements in the production of gelatin |
| US3804775A (en) * | 1970-12-25 | 1974-04-16 | Kanzaki Paper Mfg Co Ltd | Method of preparing microcapsules |
| WO1992008134A1 (en) * | 1990-10-31 | 1992-05-14 | Coulter Corporation | Biodegradable particle coatings having a protein covalently immobilized by a crosslinking agent |
| EP1063565A1 (en) * | 1999-06-24 | 2000-12-27 | Fuji Photo Film B.V. | Oil-in-water emulsions stabilised with recombinant collagen-like material |
| CN107760212A (en) * | 2017-10-19 | 2018-03-06 | 罗赛洛(温州)明胶有限公司 | A kind of manufacturing of gelatin method for reducing viscosity decline |
| CN109554120A (en) * | 2018-11-29 | 2019-04-02 | 沾化恒鑫工业科技有限公司 | A kind of method of alkaline process production cattle hide gelatin |
-
2021
- 2021-09-14 CN CN202111076057.6A patent/CN113896785B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB568182A (en) * | 1943-04-21 | 1945-03-22 | Andrew Vigodny | Improvements relating to the treatment of skin and leather materials |
| GB628757A (en) * | 1945-11-27 | 1949-09-05 | Kodak Ltd | Improvements in the production of gelatin |
| US3804775A (en) * | 1970-12-25 | 1974-04-16 | Kanzaki Paper Mfg Co Ltd | Method of preparing microcapsules |
| WO1992008134A1 (en) * | 1990-10-31 | 1992-05-14 | Coulter Corporation | Biodegradable particle coatings having a protein covalently immobilized by a crosslinking agent |
| EP1063565A1 (en) * | 1999-06-24 | 2000-12-27 | Fuji Photo Film B.V. | Oil-in-water emulsions stabilised with recombinant collagen-like material |
| CN107760212A (en) * | 2017-10-19 | 2018-03-06 | 罗赛洛(温州)明胶有限公司 | A kind of manufacturing of gelatin method for reducing viscosity decline |
| CN109554120A (en) * | 2018-11-29 | 2019-04-02 | 沾化恒鑫工业科技有限公司 | A kind of method of alkaline process production cattle hide gelatin |
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