CN103937859B - It is a kind of by raw material of bone meal by Enzymatic gelatin method - Google Patents
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Abstract
The invention belongs to technical field of preparation of gelatin, it is more particularly to a kind of by raw material of bone meal by the high-grade gelatin of Enzymatic method.The method of the present invention includes：The bone tankage of granularity≤500 μm is subjected to decalcification processing with hydrochloric acid, after being separated through solid-liquid separating machine, add water and be stirred into the bone meal of obtained decalcification and obtain slurry, plus the pH value of inorganic acid regulation slurry rear plus protease between 1.5~5 is digested, after to enzymolysis alkaline aqueous solution is added in gained slurries, the pH of slurries is adjusted so that the protease inactivation added, heating is stripped, obtain the mixed slurry containing gelatin, separation of solid and liquid is carried out through solid-liquid separating machine, obtain gelatin clear solution, again through filtering, desalination, ion exchange, concentrate and dry, obtain high-quality gelatin product.
Description
Technical field
The invention belongs to technical field of preparation of gelatin, more particularly to one kind produces top grade using bone meal as raw material by mode of action
The method of gelatin.
Background technology
It, by a kind of protein for degrading, extract, obtaining from the connective tissues such as the bone and skin of animal, is collagen that gelatin, which is,
Product after degraded, is mainly used in the fields such as capsule, food additives.Bone gelatin is the gelatin extracted from Animal Bone, its
Extracting method continues to use traditional alkali process always, and basic procedure includes：Pickling, washing, liming, washing, neutralization, wash, take out
The process such as put forward, filter, evaporating, drying.Pickling, the liming of this process need 60~100 day time to extracting, production week
Phase is very long, and this conventional method also has water consumption greatly in addition, and gelatin per ton about consumes 1000 tons of water；Waste residue, wastewater discharge
Greatly, it is seriously polluted；Investment is big, it is more to take up an area；Production automation level is low, unstable product quality；And good glue rate is low（<60%）
The shortcomings of.
In view of above traditional soda produces the shortcoming of gelatin, the production for carrying out bone gelatin using enzymolysis process technology has turned into
The focus that various countries are competitively developed.The manufacturing of gelatin enterprises such as Kodak of the U.S., France ROUSSELOT, Germany DGF have carried out correlation and ground
Study carefully, domestic Beijing University of Chemical Technology, Southern Yangtze University, Northwest Plateau-organisms Research Inst. of Chinese Academy of Sciences, the rich former limited public affairs of gelatin in Bangbu
Department etc. has also all carried out the research work of enzyme process gelatin technique.From nearest research investigation display, enzyme process gelatine technology is broadly divided into
Two kinds, it is a kind of be the bone meal obtained after being ground using skeletal grain as raw material, another is using the decalcification ossein after skeletal grain pickling as raw material.
In terms of the academic documents delivered, wherein using bone meal to be unable to reach glue,medicinal for the gelatin product that the enzymolysis process of raw material is obtained
The requirement of capsule gelatin, and the terminal that production gelatin often has production technology by raw material of decalcification ossein is difficult to control and existed not
The problem of being mass produced.
Ossein enzyme process is proposed in Chinese patent 94191461.5,200710018541.7 and 201010557127.5
The production technology of gelatin is produced, is characterized in obtaining ossein after skeletal grain pickling, and then the process such as is digested, extracted and obtains bright
Glue, because pickling process still has, therefore pickling cycle length, pickling waste water etc. it is many problem of still exist, and gained is bright
The viscosity index of glue product limits it and is widely applied also below capsule for medicine gelatin.
Bone meal enzymatic isolation method is proposed in Chinese patent 02149349.9,02125447.8 and 201110225294.4 to produce
The production technology of gelatin, the production technology is characterized in wear into skeletal grain using the form of wet-milling or dry grinding to carry out enzyme after powdery
Solution, feature is that the production cycle is shorter, and wastewater flow rate is less compared to ossein enzyme process, but the gelatin product described in above-mentioned patent
Viscosity can not equally meet the requirement of capsule for medicine gelatin product.
The content of the invention
It is an object of the invention to provide one kind using bone meal as raw material, the method that high-grade gelatin is produced by mode of action, institute
The standard of pharmagel can be reached by obtaining gelatin.
The present invention's is comprised the steps of by the method for Enzymatic gelatin by raw material of bone meal：
（1）Degreased bone grain is ground（It can be ground with grinder）Into the bone tankage of granularity≤500 μm；
（2）By step（1）The bone tankage of obtained granularity≤500 μm carries out the laggard water-filling of decalcification processing with hydrochloric acid and washed
（It is preferred that the consumption of hydrochloric acid is 1~8 times of dry bone tankage weight）, then carry out separation of solid and liquid with solid-liquid separating machine；
（3）To step（2）Add water and be stirred in the bone meal of the decalcification obtained after separation of solid and liquid（It is preferred that amount of water is dry
2 times of the bone meal weight of decalcification~7 times）, obtain slurry, then add inorganic acid regulation gained slurry pH value 1.5~5 it
Between, add protease to be digested in the slurry between 1.5~5 to pH value（The addition of preferred protease is the bone of dry decalcification
The 0.05 of powder weight~3 ‰）；
（4）To step（3）Alkaline aqueous solution is added in gained slurries after enzymolysis, the pH of slurries is adjusted so that step（3）Institute
The protease inactivation (pH of slurries is preferably adjusted to 5.5~12) of addition；Then heating is stripped（It is preferred that heating is carried out
The temperature of extracting is 45~90 DEG C）, the mixed slurry containing gelatin is obtained, separation of solid and liquid is carried out with solid-liquid separating machine；
（5）By step（4）The gelatin clear solution obtained after separation of solid and liquid is again through filtering（It can be filtered using cottonseed cake）、
Desalination, ion exchange, concentration and drying, obtain high-quality gelatin product.The high-quality gelatin production of gained meets pharmagel
Standard, Gel strength >=240g of gained gelatin, Bo Shi viscosity >=4.5mPas.
In the present invention, to step（4）Further add water and be stirred in the solid obtained after separation of solid and liquid, Ran Houjin
Row heating extracting（It is preferred that it is 65~100 DEG C to heat the temperature being stripped.It is preferred that heat time for being stripped for 1 hour~
24 hours）, the mixed slurry containing gelatin can be obtained, separation of solid and liquid is carried out with solid-liquid separating machine；What is obtained after separation of solid and liquid is bright
Glue clear solution is again through filtering（It can be filtered using cottonseed cake）, desalination, ion exchange, concentration and dry, obtain gelatin product.
Gained gelatin product meets edible gelatin standard, Gel strength >=180g of gained gelatin, Bo Shi viscosity >=3.0mPas.
Step（2）The described time for carrying out decalcification processing with hydrochloric acid is preferably 20 minutes~10 hours.
Step（2）Described in hydrochloric acid mass concentration be 0.1%~10%.
Step（3）Described in one kind in hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid of inorganic acid.
Step（3）Described in plus temperature that protease is when being digested be preferably 10~60 DEG C, the time of enzymolysis is preferred
For 15 minutes~3 days.
Described protease is pepsin, acid protease or their mixture.
Step（4）Described in alkaline aqueous solution to be selected from sodium hydrate aqueous solution, calcium hydroxide aqueous solution, sodium carbonate water-soluble
One kind in liquid, ammonium hydroxide aqueous solution etc..
Step（4）Described in time for being stripped of heating be preferably 15 minutes~48 hours.
Described desalination, preferably carries out desalination using membrane filter system.
Described ion exchange is to carry out ion exchange using anion-cation exchange resin post, and cationic ion-exchange resin can be
001 × 7 type storng-acid cation exchange resin, anion exchange resin can be 201 × 7 type strong-base anion-exchange resins.
One or more of combinations of the described solid-liquid separating machine in slag extractor, centrifuge, filter.
One aspect of the present invention can prepare the gelatin product for meeting pharmagel standard, and congealing for its gained gelatin is strong
Degree >=240g, Bo Shi viscosity >=4.5mPas disclosure satisfy that quality requirement of the capsule for medicine production to gelatin.The present invention is another
Aspect can also meet the solid material system obtained after the gelatin clear solution of pharmagel standard using solid-liquid separation
The standby gelatin product for meeting edible gelatin standard, Gel strength >=180g of its gained gelatin, Bo Shi viscosity >=3.0mPas.
Brief description of the drawings
Fig. 1 the present invention by raw material of bone meal by Enzymatic gelatin method process flow diagram.
Embodiment
Embodiment 1
Refer to Fig. 1.
（1）Degreased bone grain is ground to form to the bone tankage of granularity≤500 μm with grinder；
（2）By step（1）The bone tankage 1000g mass concentrations of obtained granularity≤500 μm are 0.1% hydrochloric acid
8000ml carries out decalcification and handled 10 hours, and separation of solid and liquid is carried out with centrifuge after then being washed；
（3）To step（2）7000ml water is added in the bone meal of the decalcification obtained after separation of solid and liquid and is stirred, is starched
Expect, then the pH value of addition acetic acid regulation gained slurry is 5, into the slurry that pH value is 5, addition is the bone meal weight of dry decalcification
3 ‰ acid protease carries out enzymolysis 15 minutes, and temperature during enzymolysis is 60 DEG C；
（4）To step（3）Aqueous sodium carbonate is added in gained slurries after enzymolysis, the pH for adjusting slurries is 5.5 so that step
Suddenly（3）The acid protease inactivation added；Then it is stripped 15 minutes in the case where temperature is 90 DEG C, obtains mixed containing gelatin
Slurry is closed, separation of solid and liquid is carried out with centrifuge；
（5）By step（4）The gelatin clear solution obtained after separation of solid and liquid is after cottonseed cake is filtered, using milipore filter
Filter plant carries out desalination, then carries out ion exchange through anion-cation exchange resin post（Cationic ion-exchange resin is 001 × 7 type
Storng-acid cation exchange resin, anion exchange resin is 201 × 7 type strong-base anion-exchange resins）, then again through dense
Contract and dry, obtain meeting the high-quality gelatin product of pharmagel standard.
To step（4）Add water and 3000ml and be stirred in the solid obtained after separation of solid and liquid, be then 100 DEG C in temperature
Under be stripped 1 hour, obtain the mixed slurry containing gelatin, separation of solid and liquid carried out with centrifuge；Obtained after separation of solid and liquid
Gelatin clear solution carries out desalination after cottonseed cake is filtered using ultrafiltration membrance filter equipment, then through cation and anion exchange tree
Fat post carries out ion exchange（Cationic ion-exchange resin is 001 × 7 type storng-acid cation exchange resin, anion exchange resin
For 201 × 7 type strong-base anion-exchange resins）, it is then concentrated again and dry, obtain meeting the gelatin of edible gelatin standard
Product.
According to People's Republic of China (PRC) light industry standard QB2354-2005 tested obtained by meet pharmagel standard
High-quality gelatin product, as a result as shown in table 1.
Table 1
According to National Standard of the People's Republic of China GB6783-94 tested obtained by meet the gelatin of edible gelatin standard
Product, as a result as shown in table 2.
Table 2
Embodiment 2
Refer to Fig. 1.
（1）Degreased bone grain is ground to form to the bone tankage of granularity≤500 μm with grinder；
（2）By step（1）The bone tankage 1000g mass concentrations of obtained granularity≤500 μm are 0.1% hydrochloric acid
1000ml carries out decalcification and handled 20 minutes, and separation of solid and liquid is carried out with slag extractor after then being washed；
（3）To step（2）2000ml water is added in the bone meal of the decalcification obtained after separation of solid and liquid and is stirred, is starched
Expect, then the pH value of addition hydrochloric acid regulation gained slurry is 1.5, into the slurry that pH value is 1.5, addition is the bone meal of dry decalcification
The pepsin of weight 0.05 ‰ carries out enzymolysis 3 days, and temperature during enzymolysis is 10 DEG C；
（4）To step（3）Sodium hydrate aqueous solution is added in gained slurries after enzymolysis, the pH for adjusting slurries is 12 so that step
Suddenly（3）The pepsin inactivation added；Then it is stripped 10 hours in the case where temperature is 45 DEG C, obtains the mixing containing gelatin
Slurry, separation of solid and liquid is carried out with slag extractor；
（5）By step（4）The gelatin clear solution obtained after separation of solid and liquid is after cottonseed cake is filtered, using milipore filter
Filter plant carries out desalination, then carries out ion exchange through anion-cation exchange resin post（Cationic ion-exchange resin is 001 × 7 type
Storng-acid cation exchange resin, anion exchange resin is 201 × 7 type strong-base anion-exchange resins）, then again through dense
Contract and dry, obtain meeting the high-quality gelatin product of pharmagel standard.
To step（4）Add water and 5000ml and be stirred in the solid obtained after separation of solid and liquid, be then 65 DEG C in temperature
Under be stripped 24 hours, obtain the mixed slurry containing gelatin, separation of solid and liquid carried out with slag extractor；Obtained after separation of solid and liquid
Gelatin clear solution carries out desalination after cottonseed cake is filtered using ultrafiltration membrance filter equipment, then through cation and anion exchange tree
Fat post carries out ion exchange（Cationic ion-exchange resin is 001 × 7 type storng-acid cation exchange resin, anion exchange resin
For 201 × 7 type strong-base anion-exchange resins）, it is then concentrated again and dry, obtain meeting the gelatin of edible gelatin standard
Product.
According to People's Republic of China (PRC) light industry standard QB2354-2005 tested obtained by meet pharmagel standard
High-quality gelatin product, as a result as shown in table 3.
Table 3
According to National Standard of the People's Republic of China GB6783-94 tested obtained by meet the gelatin of edible gelatin standard
Product, as a result as shown in table 4.
Table 4
Embodiment 3
Refer to Fig. 1.
（1）Degreased bone grain is ground to form to the bone tankage of granularity≤500 μm with grinder；
（2）By step（1）The bone tankage 1000g mass concentrations of obtained granularity≤500 μm are 5% hydrochloric acid
4000ml carries out decalcification and handled 5 hours, and separation of solid and liquid is carried out with slag extractor and filter after then being washed；
（3）To step（2）3500ml water is added in the bone meal of the decalcification obtained after separation of solid and liquid and is stirred, is starched
Expect, then the pH value of addition phosphoric acid regulation gained slurry is 3.0, into the slurry that pH value is 3.0, addition is the bone meal of dry decalcification
The pepsin of weight 0.5 ‰ and 1.0 ‰ acid protease carry out enzymolysis 36 hours, and temperature during enzymolysis is 35 DEG C；
（4）To step（3）Calcium hydroxide aqueous solution is added in gained slurries after enzymolysis, the pH for adjusting slurries is 9 so that step
Suddenly（3）Pepsin and the acid protease inactivation added；Then it is stripped 24 hours, is contained in the case where temperature is 50 DEG C
There is the mixed slurry of gelatin, separation of solid and liquid is carried out with slag extractor and filter；
（5）By step（4）The gelatin clear solution obtained after separation of solid and liquid is after cottonseed cake is filtered, using milipore filter
Filter plant carries out desalination, then carries out ion exchange through anion-cation exchange resin post（Cationic ion-exchange resin is 001 × 7 type
Storng-acid cation exchange resin, anion exchange resin is 201 × 7 type strong-base anion-exchange resins）, then again through dense
Contract and dry, obtain meeting the high-quality gelatin product of pharmagel standard.
To step（4）Add water and 1000ml and be stirred in the solid obtained after separation of solid and liquid, be then 75 DEG C in temperature
Under be stripped 6 hours, obtain the mixed slurry containing gelatin, separation of solid and liquid carried out with slag extractor and filter；Separation of solid and liquid
The gelatin clear solution obtained afterwards after cottonseed cake is filtered, using ultrafiltration membrance filter equipment carry out desalination, then through negative and positive from
Sub-exchange resin post carries out ion exchange（Cationic ion-exchange resin is 001 × 7 type storng-acid cation exchange resin, anion
Exchanger resin is 201 × 7 type strong-base anion-exchange resins）, it is then concentrated again and dry, obtain meeting edible gelatin mark
Accurate gelatin product.
According to People's Republic of China (PRC) light industry standard QB2354-2005 tested obtained by meet pharmagel standard
High-quality gelatin product, as a result as shown in table 5.
Table 5
According to National Standard of the People's Republic of China GB6783-94 tested obtained by meet the gelatin of edible gelatin standard
Product, as a result as shown in table 6.
Table 6
Claims (2)
1. it is a kind of by raw material of bone meal by Enzymatic gelatin method, it is characterized in that, described method is comprised the steps of：
(1) degreased bone grain is ground to form to the bone tankage of granularity≤500 μm；
(2) bone tankage for granularity≤500 μm for obtaining step (1) is used dense for 1~8 times of quality of dry bone tankage weight
The hydrochloric acid spent for 0.1%~10% carries out decalcification processing laggard water-filling in 20 minutes~10 hours and washed, and is then entered with solid-liquid separating machine
Row separation of solid and liquid；
(3) add water and be stirred into the bone meal of the decalcification obtained after step (2) separation of solid and liquid, obtain slurry, its amount of water
For 2 times~7 times of the bone meal weight of dry decalcification；Then the pH value of inorganic acid regulation gained slurry is added between 1.5~5, to
0.05~3 ‰ protease that pH value adds the bone meal weight for being dry decalcification in the slurry between 1.5~5 is digested, institute
The temperature for the enzymolysis stated is 10~60 DEG C, and the time of enzymolysis is 15 minutes~3 days；
The one kind of described inorganic acid in hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid；
(4) alkaline aqueous solution is added in gained slurries after being digested to step (3), the pH of slurries is adjusted for 5.5~12 so that step
(3) the protease inactivation added；Then heating is stripped, and is obtained the mixed slurry containing gelatin, is entered with solid-liquid separating machine
Row separation of solid and liquid；Wherein, the temperature that described heating is stripped is 45~90 DEG C；
Described alkaline aqueous solution is selected from sodium hydrate aqueous solution, calcium hydroxide aqueous solution, aqueous sodium carbonate, ammonium hydroxide water
One kind in solution；
(5) the gelatin clear solution obtained after step (4) separation of solid and liquid through filtering, desalination, ion exchange, concentration and is done again
It is dry, obtain gelatin product；Gained gelatin product meets pharmagel standard, and Gel strength >=240g of gained gelatin, Bo Shi glues
Degree >=4.5mPas；
And add water and be stirred into the solid obtained after step (4) separation of solid and liquid, it is then to enter at 65~100 DEG C in temperature
Row heating extracting, obtains the mixed slurry containing gelatin, separation of solid and liquid is carried out with solid-liquid separating machine；What is obtained after separation of solid and liquid is bright
Glue clear solution through filtering, desalination, ion exchange, concentration and is dried again, obtains gelatin product；Gained gelatin product meets edible
Gelatin standard, Gel strength >=180g of gained gelatin, Bo Shi viscosity >=3.0mPas.
2. according to the method described in claim 1, it is characterized in that：Described protease be pepsin, acid protease or it
Mixture.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694605A (en) * | 2015-03-14 | 2015-06-10 | 宁夏鑫浩源明胶有限公司 | Industrial production process of gelatin for capsule prepared by using biological enzyme method |
| CN105707729A (en) * | 2016-02-14 | 2016-06-29 | 合肥学院 | Technology for preparing deer bone meal |
| CN107541537A (en) * | 2016-06-23 | 2018-01-05 | 宁夏鑫浩源生物科技股份有限公司 | Preparation of gelatin with enzyme technique |
| CN106591406B (en) * | 2016-11-23 | 2020-03-24 | 江南大学 | Method for preparing bone gelatin by using ultrasonic-assisted enzyme method |
| CN107083415A (en) * | 2017-05-27 | 2017-08-22 | 四川汇宇生物技术有限公司 | A kind of production method of gelatin |
| CN110655569B (en) * | 2019-10-29 | 2021-06-25 | 江南大学 | Method for preparing bone gelatin |
| DE102019130197A1 (en) * | 2019-11-08 | 2021-05-12 | Gelita Ag | Process for the production of bone gelatin, and produced bone gelatin |
| DE102019130196A1 (en) * | 2019-11-08 | 2021-05-12 | Gelita Ag | Process for the production of collagen peptides from bone, and produced collagen peptides |
| CN115368454B (en) * | 2022-09-30 | 2023-05-12 | 斐缦(长春)医药生物科技有限责任公司 | Gelatin and preparation method thereof |
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