CN106281049B - A kind of technique for extracting high-purity gelatin from ox-hide - Google Patents
A kind of technique for extracting high-purity gelatin from ox-hide Download PDFInfo
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- CN106281049B CN106281049B CN201610745422.0A CN201610745422A CN106281049B CN 106281049 B CN106281049 B CN 106281049B CN 201610745422 A CN201610745422 A CN 201610745422A CN 106281049 B CN106281049 B CN 106281049B
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- C09H—PREPARATION OF GLUE OR GELATINE
- C09H3/00—Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating
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Abstract
The present invention relates to a kind of from ox-hide extracts the technique of high-purity gelatin, belongs to the method in gelatin extraction.Step：Step 1 after crushing ox-hide, is added into the aqueous solution containing 1~3% potassium sulfate, 0.5~2% sodium citrate and is impregnated；Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, obtains leaching liquor by step 3；Step 4 is added modenite in leaching liquor and is adsorbed, filters feed liquid after the completion of absorption, and filtrate passes through ultrafiltration membrance filter, and the filtrate of ultrafiltration passes through nanofiltration membrane again and is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.The gelatin that the present invention is prepared has the advantages that purity is high.
Description
Technical field
The present invention relates to a kind of from ox-hide extracts the technique of high-purity gelatin, belongs to the method in gelatin extraction.
Background technique
Gelatin finished product be colourless or faint yellow, transparent or semitransparent and hard non-crystalline material, color more white matter amount more
It is good.Gelatin does not dissolve in cold water, but can slowly water swelling soften, the absorbable water for being equivalent to 5~10 times of weight of gelatin.Gelatin
The organic acids such as glycerol, acetic acid, salicylic acid and phthalic acid can be dissolved in, do not dissolve in ethyl alcohol and ether, be in thin stick or fibre structure, by
The desmachyme that duplicate peptide bond is wound in.General physics and chemical property with a- amino acid and protein.Warm water is bright
The most common solvent of glue, gelatin dissolve in hot water, form thermoreversible gels, it has extremely excellent physical property（Such as glue
Freeze power, affinity, high dispersion, low viscosity characteristics, dispersion stabilization, retentiveness, coating property, toughness and invertibity）, therefore
It is bright
Glue is a kind of important food additives, such as the jelly of food, stabilizer, thickener, foaming agent, emulsification
Agent, dispersing agent, clarifying agent etc..
The collagen rich in the connective tissues such as skin, the bone of animal, collagen are made of multiple proteins,
Collagen therein is the main component of glue, it is not soluble in water, is also insoluble in the weak solution of acid, alkali and salt.But in heat
In water under certain pH value condition, a degree of hydrolysis occurs for collagen, so that original high polymer is become low molecular weight, energy molten
In the glue with certain viscous shelf of hot water, here it is the principles of glue.Therefore, the process of high-quality gelatin and collagen is made
The intermolecular covalent cross-linking and non-covalent bond with intramolecular of stable collagenous fibres is exactly destroyed by processing method appropriate, is released
Tropocollagen molecule is released, is then broken the hydrogen bond for stablizing collagen helix also to release gelatin by heating.
CN103289576A discloses a kind of preparation method of tuna skin gelatin, belongs to stock of fish technical field of comprehensive utilization.This
Tuna skin is carried out mentioning glue by invention after preprocessed, degreasing, soda acid processing, is gone by active carbon filtering deodorant, ion exchange
Removing heavy metals ion purification after, then carry out vacuum concentration and spray drying obtain tuna skin gelatin finished product.CN101735464A
A kind of preparation method of fishskin gelatin is disclosed, preparation flow is：Fish-skin → drying → cleaning, decontamination → degreasing → removal of impurities
→ cleaning → ultra high pressure treatment → is beaten → mentions glue → centrifugation → drying → finished gelatin, and the present invention is assisted by superhigh pressure technique
Processing produces the fishskin gelatin of high-quality in conjunction with thermal extraction.
But the gelatin of above method preparation has that impurity content is high.
Summary of the invention
The purpose of the present invention is：A kind of method that gelatin is extracted from ox-hide is provided, this method can remove in ox-hide
The impurity such as fat, inorganic salts, obtained gelatin have the advantages that purity is high.
Technical solution is：
A kind of technique for extracting high-purity gelatin from ox-hide, includes the following steps：
Step 1 after crushing ox-hide, is added into the aqueous solution containing 1~3% potassium sulfate, 0.5~2% sodium citrate
It is impregnated；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and solids is filtered out
Afterwards, it is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, obtains leaching liquor by step 3；
Step 4 is added modenite in leaching liquor and is adsorbed, filters feed liquid after the completion of absorption, and filtrate is by super
Membrane filtration, the filtrate of ultrafiltration pass through nanofiltration membrane again and are concentrated, and after nanofiltration concentrate is dried, obtain gelatin.
In the step 1, the weight ratio of ox-hide and aqueous solution is 1：4~6, soaking temperature is 35~45 DEG C, when immersion
Between be 2~4h.
In the step 2, grease removal agent is petroleum ether and ethyl acetate according to weight ratio 3：1 mixture, solids with
The weight ratio of grease removal agent is 1：0.5~3；At 30~40 DEG C, soaking time is 2~4h for temperature control in soaking process.
In the step 2,3% lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide are contained in the inorganic acid aqueous solution
Weight ratio with inorganic acid aqueous solution is 1：8~10；For extraction temperature at 40~50 DEG C, extraction time is 3~6h.
In the step 4, the weight of modenite is the 1~4% of leaching liquor weight, leaching liquor temperature in adsorption process
5~15 DEG C are maintained at, needs to be stirred in adsorption process, adsorption time is 2~4h.
The modenite is modified mordenite, and method of modifying is：Modenite between 80~100 mesh is used
10% NH4Digestion 12h at 80 DEG C of Cl solution impregnates 50~100h with the HCl solution of 2mol/L, is washed in washing lotion without Cl-,
120 DEG C of drying, according still further to solid and liquid weight than 1：5 in concentrated phosphoric acid（16.03mol/L）It is dried at impregnating 7 days, 100 DEG C, moves to porcelain earthenware
Crucible is in micro-wave oven（220V, 2450MHz）Moderate heat heats 10min, is washed with water after taking out cooling, then dries at 120 DEG C, is changed
Sex pilus geolyte.
In the step 4, the molecular cut off of ultrafiltration membrane is 200kDa~400kDa, and the molecular cut off of nanofiltration membrane is
300Da~500Da.
Beneficial effect
The gelatin that the present invention is prepared has the advantages that purity is high.
Specific embodiment
Percentage in the present invention all refers to weight percent in no special instruction.
Embodiment 1
Step 1 after crushing ox-hide, is added into the aqueous solution containing 1% potassium sulfate, 0.5% sodium citrate and is soaked
The weight ratio of bubble, ox-hide and aqueous solution is 1：4, soaking temperature is 35 DEG C, and soaking time is 2h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether
With ethyl acetate according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1：0.5；Temperature in soaking process
At 30 DEG C, soaking time is 2h for control, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, contains 3% in the inorganic acid aqueous solution by step 3
The weight ratio of lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1：8；Extraction temperature is at 40 DEG C, extraction
Time is 3h, obtains leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 1% of leaching liquor weight,
Leaching liquor temperature is maintained at 5 DEG C in adsorption process, needs to be stirred in adsorption process, and adsorption time is 2h, after the completion of absorption
Feed liquid is filtered, filtrate is 200kDa ultrafiltration membrance filter by molecular cut off, and the filtrate of ultrafiltration is again by molecular cut off
300Da nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.
Embodiment 2
Step 1 after crushing ox-hide, is added into the aqueous solution containing 3% potassium sulfate, 2% sodium citrate and is impregnated,
The weight ratio of ox-hide and aqueous solution is 1：6, soaking temperature is 45 DEG C, and soaking time is 4h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether
With ethyl acetate according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1： 3；Temperature control in soaking process
For system at 40 DEG C, soaking time is 4h, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, contains 3% in the inorganic acid aqueous solution by step 3
The weight ratio of lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1： 10；Extraction temperature is at 50 DEG C, leaching
Mentioning the time is 6h, obtains leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 4% of leaching liquor weight,
Leaching liquor temperature is maintained at 15 DEG C in adsorption process, needs to be stirred in adsorption process, and adsorption time is 4h, after the completion of absorption
Feed liquid is filtered, filtrate is 400kDa ultrafiltration membrance filter by molecular cut off, and the filtrate of ultrafiltration is again by molecular cut off
500Da nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.
Embodiment 3
Step 1 after crushing ox-hide, is added into the aqueous solution containing 2% potassium sulfate, 1% sodium citrate and is impregnated,
The weight ratio of ox-hide and aqueous solution is 1：5, soaking temperature is 40 DEG C, and soaking time is 3h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether
With ethyl acetate according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1：2；Temperature control in soaking process
For system at 35 DEG C, soaking time is 3h, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, contains 3% in the inorganic acid aqueous solution by step 3
The weight ratio of lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1：9；Extraction temperature is at 45 DEG C, extraction
Time is 4h, obtains leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 2% of leaching liquor weight,
Leaching liquor temperature is maintained at 10 DEG C in adsorption process, needs to be stirred in adsorption process, and adsorption time is 3h, after the completion of absorption
Feed liquid is filtered, filtrate is 300kDa ultrafiltration membrance filter by molecular cut off, and the filtrate of ultrafiltration is again by molecular cut off
400Da nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.
Embodiment 4
Difference with embodiment 3 is：Modenite refers to that modified mordenite, method of modifying are：By 80~100 mesh it
Between modenite with 10% NH4Digestion 12h at 80 DEG C of Cl solution impregnates 50~100h, washing with the HCl solution of 2mol/L
Into washing lotion without Cl-, 120 DEG C of drying, according still further to solid and liquid weight than 1：5 in concentrated phosphoric acid（16.03mol/L）It impregnates 7 days, 100 DEG C
Lower drying, moves to porcelain crucible in micro-wave oven（220V, 2450MHz）Moderate heat heats 10min, is washed with water after taking out cooling, then
120 DEG C of drying, obtain modified mordenite.
Step 1 after crushing ox-hide, is added into the aqueous solution containing 2% potassium sulfate, 1% sodium citrate and is impregnated,
The weight ratio of ox-hide and aqueous solution is 1：5, soaking temperature is 40 DEG C, and soaking time is 3h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether
With ethyl acetate according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1：2；Temperature control in soaking process
For system at 35 DEG C, soaking time is 3h, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, contains 3% in the inorganic acid aqueous solution by step 3
The weight ratio of lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1：9；Extraction temperature is at 45 DEG C, extraction
Time is 4h, obtains leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 2% of leaching liquor weight,
Leaching liquor temperature is maintained at 10 DEG C in adsorption process, needs to be stirred in adsorption process, and adsorption time is 3h, after the completion of absorption
Feed liquid is filtered, filtrate is 300kDa ultrafiltration membrance filter by molecular cut off, and the filtrate of ultrafiltration is again by molecular cut off
400Da nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.
Reference examples 1
Difference with embodiment 3 is：Potassium sulfate is not added in the soaking technology of step 1.
Step 1 after crushing ox-hide, is added into the aqueous solution containing 1% sodium citrate and is impregnated, ox-hide and water
The weight ratio of solution is 1：5, soaking temperature is 40 DEG C, and soaking time is 3h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether
With ethyl acetate according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1：2；Temperature control in soaking process
For system at 35 DEG C, soaking time is 3h, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts, contains 3% in the inorganic acid aqueous solution by step 3
The weight ratio of lactic acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1：9；Extraction temperature is at 45 DEG C, extraction
Time is 4h, obtains leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 2% of leaching liquor weight,
Leaching liquor temperature is maintained at 10 DEG C in adsorption process, needs to be stirred in adsorption process, and adsorption time is 3h, after the completion of absorption
Feed liquid is filtered, filtrate is 300kDa ultrafiltration membrance filter by molecular cut off, and the filtrate of ultrafiltration is again by molecular cut off
400Da nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin.
Gelatin product is detected according to GB 6783-2013, as a result as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Reference examples 1 | |
| Collagen content % | 87.5 | 87.4 | 86.6 | 88.9 | 84.2 |
| Ash content % | 0.4 | 0.5 | 0.4 | 0.2 | 0.4 |
| Fatty % | 0.09 | 0.08 | 0.07 | 0.06 | 0.07 |
| Water-insoluble % | 0.08 | 0.08 | 0.11 | 0.08 | 0.16 |
| Gelatin gel strength g | 485 | 492 | 481 | 510 | 471 |
As can be seen from the table, the gelatin that method of the invention obtains has the advantages that purity is high, wherein protein content it is high,
Fat content is small.By being modified to modenite in embodiment 4, it can be improved for the adsorption capacity of impurity, makes ash
Content is divided to reduce；Embodiment 3 joined potassium sulfate in preparatory soaking cycle for reference examples 1, can promote ox-hide
The dispersion of middle tissue makes fat be easier to be removed in grease removal operation, improves purity.
Claims (1)
1. a kind of technique for extracting high-purity gelatin from ox-hide, which is characterized in that include the following steps：
Step 1 after crushing ox-hide, is added into the aqueous solution containing 2% potassium sulfate, 1% sodium citrate and is impregnated, ox-hide
Weight ratio with aqueous solution is 1：5, soaking temperature is 40 DEG C, and soaking time is 3h；
Step 2 filters out solids in the feed liquid of step 1, and addition is impregnated into grease removal agent, and grease removal agent is petroleum ether and second
Acetoacetic ester is according to weight ratio 3：The weight ratio of 1 mixture, solids and grease removal agent is 1：2；Temperature control exists in soaking process
35 DEG C, soaking time is 3h, after solids is filtered out, is evaporated under reduced pressure and removes solvent, obtain grease removal ox-hide；
Grease removal ox-hide is added in inorganic acid aqueous solution and extracts by step 3, and 3% cream is contained in the inorganic acid aqueous solution
The weight ratio of acid, 4% acetic acid, 2% citric acid, grease removal ox-hide and inorganic acid aqueous solution is 1：9；Extraction temperature is at 45 DEG C, extraction
Between be 4h, obtain leaching liquor；
Step 4 is added modenite in leaching liquor and is adsorbed, and the weight of modenite is the 2% of leaching liquor weight, absorption
Leaching liquor temperature is maintained at 10 DEG C in the process, needs to be stirred in adsorption process, and adsorption time is 3h, will material after the completion of absorption
Liquid filtering, filtrate are 300kDa ultrafiltration membrance filters by molecular cut off, and it is 400Da that the filtrate of ultrafiltration passes through molecular cut off again
Nanofiltration membrane is concentrated, and after nanofiltration concentrate is dried, obtains gelatin；
The modenite refers to that modified mordenite, method of modifying are：By the modenite between 80~100 mesh with 10%
NH4Digestion 12h at 80 DEG C of Cl solution impregnates 50~100h with the HCl solution of 2mol/L, is washed in washing lotion without Cl-, 120 DEG C
Drying, according still further to solid and liquid weight than 1：5 dry at 16.03mol/L concentrated phosphoric acid is impregnated 7 days, 100 DEG C, move to porcelain crucible and exist
The microwave ingle of 220V, 2450MHz heat 10min, are washed with water after taking out cooling, then dry at 120 DEG C, obtain modified silk
Geolyte
The percentage refers to weight percent.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286252A (en) * | 2011-06-21 | 2011-12-21 | 郭小棋 | Process for producing gelatin by using acid method |
| CN104087641A (en) * | 2014-07-08 | 2014-10-08 | 天津大学 | Yak skin blood pressure-decreasing collagen polypeptide and preparation method thereof |
| WO2014209101A3 (en) * | 2013-06-28 | 2015-03-05 | Universiti Putra Malaysia | Method of obtaining gelatin from aquatic animals |
| CN104479567A (en) * | 2014-10-27 | 2015-04-01 | 浙江吉达生物科技有限公司 | After-extraction method of medicinal cow leather gelatin |
-
2016
- 2016-08-29 CN CN201610745422.0A patent/CN106281049B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286252A (en) * | 2011-06-21 | 2011-12-21 | 郭小棋 | Process for producing gelatin by using acid method |
| WO2014209101A3 (en) * | 2013-06-28 | 2015-03-05 | Universiti Putra Malaysia | Method of obtaining gelatin from aquatic animals |
| CN104087641A (en) * | 2014-07-08 | 2014-10-08 | 天津大学 | Yak skin blood pressure-decreasing collagen polypeptide and preparation method thereof |
| CN104479567A (en) * | 2014-10-27 | 2015-04-01 | 浙江吉达生物科技有限公司 | After-extraction method of medicinal cow leather gelatin |
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Effective date of registration: 20180925 Address after: 318050 six 14 District 27, Zhong Lin village, Xinqiao Town, Luqiao District, Taizhou, Zhejiang. Applicant after: Luo Xianfeng Address before: 610000 Xinhua Xinhua 4 group, Chengdu high tech Zone, Sichuan Applicant before: Qian Yulian |
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Effective date of registration: 20190809 Address after: 322000 Chengshan Road, Chian Special Industrial Park, Yiwu City, Jinhua City, Zhejiang Province Patentee after: Zhejiang Hefeng Rubber Industry Co., Ltd. Address before: 318050 six village, 14 District 27, Xinqiao village, Xinqiao Town, Luqiao District, Zhejiang, Taizhou Patentee before: Luo Xianfeng |