CN101107974A - Method of preparing edible gelatin with combined zyme - Google Patents
Method of preparing edible gelatin with combined zyme Download PDFInfo
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- CN101107974A CN101107974A CNA2007100185417A CN200710018541A CN101107974A CN 101107974 A CN101107974 A CN 101107974A CN A2007100185417 A CNA2007100185417 A CN A2007100185417A CN 200710018541 A CN200710018541 A CN 200710018541A CN 101107974 A CN101107974 A CN 101107974A
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Abstract
The invention provides a method using combined degradation ossein adopting prolease of different specificities in sequence for zymolysis to prepare edible gelatine. The detailed procedure is that: marinating the ossein washed by dipping into acid water of the traditional lie wash technics into water for 2h to 3h, adding acid protease with the quality of dry ossein achieves to 1 per mill to 3 per mill after oil removal and conducting the first deterioration 2 to 5 when the temperature is 55 DEG C. to 60 DEG C.; raising mucus, filtering and drying after sterilizing enzyme with high temperature, thus achieving the dry gelatin; then adding water in the remained ossein, adjusting the solution reacted with the PH reaches to 4 to 8 by using alkali; then adding neutral or alkaline protease with the quality of the original dry ossein as 2 to 3 per mill and conducting the second deterioration with the temperature of 55 to 60 DEG C.; then raising mucus, filtering and drying after sterilizing enzyme with high temperature, thus achieving the dry gelatin. The ossein consumption for the first zymohydrolysis of the invention achieves 60 per cent per cent to 80 per cent and the viscosity of the glutin obtained is 2.3 mPa is multiplied by s and the bloom is 139 Bloom g; while the ossein consumption for the second zymohydrolysis of the invention achieves 15 to 30 per cent with the viscosity reaches to 3.4 mPa is multiplied by s and bloom of 101 Bloom g. Only little amoune of soft ossein dregs without viscosity are remained after boiled the remained ossein.
Description
Technical field
The present invention relates to a kind of preparation method of gelatin, relate in particular to a kind of method of utilizing combination enzyme degrading ossein to prepare edible gelatin.
Background technology
When the digital age impacted to photographic gelatin, the market demand of medicine and edible gelatin was but progressively enlarging; Because the functional and safe handling property problem of gelatin receives increasing concern, this is with regard to the further raising of inevitable requirement gelatin quality simultaneously.In the prior art, the alkali process production cycle is long, the liming operation reaches 40~60 days, production efficiency is lower, environmental pollution is comparatively serious, and the gelatin product selectivity of producing is not strong, and removing the more share of edible gelatin is photographic gelatin and pharmagel, and this preparation to edible gelatin is quite restriction.Acid technological process then more is used for cladding, the less aggregate that is used for, and stronger to the contaminative of environment.Thereby also required the improvement of gelatin technology.
From the fifties in last century, people are introduced into the degradation of enzyme to collagen in the preparation of gelatin technology with regard to attempting.Since more than half a century, the researcher has obtained very big remarkable achievement.But up to the present, also rarely have process application in the big production of gelatin, this difficulty to control with the enzymolysis collagen reaction is relevant.
Chinese patent CN1473901A openly adopts the clay method that is equipped with gelatin of bone of single not demineralization of enzyme degraded degreasing, not demineralization of degreasing has just reduced the pickling link, conserve water resource, but the process that aggregate the is worn into bone mud skeletal grain of traditional handicraft preparation having increased cost relatively then; And single enzyme degraded, the bone gelatin PD is incomplete, and remaining bone slag need return reaction pot extracting again again, may the quality of follow-up gelatin be influenced to some extent.The method product is primarily aimed at pharmagel.
Summary of the invention
The object of the present invention is to provide a kind of with short production cycle, product quality is comparatively single-minded, utilize combination enzyme degrading ossein to prepare the method for edible gelatin.
Enzyme is a biocatalyst, has the selectivity of height, the action site difference of promptly different protease peptide chains.Therefore adopt the different protease of selectivity successively the compound mode degrade collagen of enzymolysis prepare gelatin, both increased the enzymolysis site, aggregate is degraded as far as possible finishes, do not need to return again and handle, reduced subsequent handling and destabilizing factor; Again with the enzymolysis process separation of two kinds of enzymes, make the gelatin peptide of small component produce less simultaneously.The present invention utilizes this principle, and the mode that adopts acid protease and neutrality or slight alkaline protease to degrade respectively shortens the manufacturing of gelatin cycle to reach, prepares viscosity, freezes the edible gelatin level that the power index is up to state standards and requires.
The present invention adopts combination enzyme degrading ossein to prepare the method for edible gelatin, comprises following processing step:
1. with the ossein after traditional alkali process pickling washing, steeped oil removing 2~3 hours with the water logging of 2~3 times of volumes.
The pickling of tradition alkali process prepares the technology of ossein:------------pickling---washing---drying, the skeletal grain size of ossein is 10~50mm to the gelatine raw material after the pickling in the skeletal grain sorting in degreasing to pound bone.
2. the acid protease that adds dried ossein quality 1~3 ‰, carry out the degraded first time under 55~60 ℃: the degradation reaction time is 2~3 hours, heat up rapidly then,, use pH value of solution to 6~7 behind the alkali conditioned reaction then in 85~100 ℃ of following inactivator 20~30Min.Acid protease can adopt pepsin or cathepsin; Regulating with alkali is NaOH, calcium hydroxide or ammonium hydroxide.
3. under 50~60 ℃ of temperature, carry glue, filter glue, dry gelatin dry.
Gelatin solution detects after drying, and the viscosity of the gelatin of enzymolysis acquisition for the first time is 2.3~2.7mPas, freezes power 139~197Bloom g; Consume bone amount 60~80%; Estimation glue yield rate 51~68%.
4. in remaining ossein, add water, the bone water volume ratio was controlled at 1: 2.5~1: 3; With pH value of solution to 4~8 behind the alkali conditioned reaction, add the neutrality or the slight alkaline protease of former dried ossein quality 1~3 ‰ again, carry out the degraded second time under 55~60 ℃: enzyme digestion reaction 2~3 hours is warming up to 85~100 ℃ of deactivation 20~30min then rapidly.
Wherein, neutral proteinase can adopt the AS1.398 neutral proteinase, and slight alkaline protease can adopt 2701 alkali proteases, trypsase or papain; Regulating with alkali is NaOH, calcium hydroxide or ammonium hydroxide.
5. under 50~60 ℃ of temperature, carry glue, filter glue, dry gelatin dry;
The gained gelatin solution detects after drying, and the viscosity of the gelatin of enzymolysis acquisition for the second time is 2.2~3.4mPas, and freezing power is 101~168Bloom g; Consume bone amount 15~30%, estimation glue yield rate 13.5~27%.
6. remaining a small amount of ossein adds the water temperature that raises, and boils hydrolysis, and is only surplus a small amount of soft and do not have a bone slag of viscosity.
The present invention compared with prior art has the following advantages:
1, the present invention adopts the different protease of selectivity---and the ossein after acid protease and neutrality or slight alkaline protease are washed traditional alkali process pickling makes up enzymolysis by the mode that adds successively, both increased the enzymolysis site, aggregate is degraded as far as possible to finish, do not need to return again and handle, reduced subsequent handling and destabilizing factor; Again with the enzymolysis process separation of two kinds of enzymes, make the gelatin peptide generation of small component less simultaneously, obtained the comparatively single-minded edible gelatin of quality.
2, the present invention is replaced the liming operation in traditional alkaline process by the enzymolysis operation, when reducing process variations, has shortened the production cycle of gelatin, has reduced environmental pollution.
The specific embodiment
Embodiment 1, with ossein adopt ossein after the traditional alkali process pickling washing (skeletal grain 30~50mm, pH4~5, ossein water content 62.3%) 5.44kg makes up the enzymolysis experiment:
Add ossein triplication water logging bubble 2 hours, and ossein was expanded, and remove grease, add the pepsin of ossein quality 2.65 ‰, be warming up to 60 ℃, carry out the enzymolysis first time; Behind the enzymolysis 2 hours, be warming up to 85 ℃ rapidly, keep high temperature 30min, make enzyme-deactivating, use again behind the NaOH conditioned reaction behind pH value of solution to 6~7, under 60 ℃, carry glue 2h, consume bone amount 60~80%, estimation glue yield rate 51~68%.
The water that in remaining ossein, adds the triplication volume, and about the pH to 6 with the NaOH regulation system; The AS1.398 neutral proteinase that adds green bone quality amount 2.65 ‰ again carries out the enzymolysis second time under 60 ℃ of temperature; Behind the enzymolysis 2 hours, be warming up to 85 ℃ rapidly, keep high temperature 30min, make enzyme-deactivating; Under 60 ℃, carry glue 2h then, consume bone amount 15~30% (estimation glue yield rate 13.5~27%);
Double in the surplus bone water boil of volume is only surplus a small amount of soft and do not have a bone slag of viscosity.
The glue drying gets wafer, viscosimetric, the power of freezing after each extracting.After testing, the viscosity that obtains the enzymolysis gelatin first time is 2.3mPas, freezes power 139Bloom g; The viscosity of enzymolysis glue is 3.4mPas for the second time, and freezing power is 101Bloom g.
Embodiment 2, ossein is adopted ossein (skeletal grain 10~20mm, pH4~5) 100kg after the traditional alkali process pickling washing, add the water logging bubble 3 hours of 3 times of amounts of ossein volume, ossein is expanded; After the oil removing, add the pepsin of ossein amount 1.5 ‰, the enzymolysis first time is carried out in heating and cooling to 60 ℃; Behind the enzymolysis 3 hours, be warming up to 90 ℃ rapidly, keep high temperature 20min, make enzyme-deactivating, use pH value of solution to 6~7 behind the calcium hydroxide conditioned reaction again, carry glue 2h in 60 ℃ then, the glue yield rate that obtains the enzymolysis gelatin first time after the glue drying is 30~35%, and viscosity 2.5mPas freezes power 189Bloom g.
Add the long-pending water of surplus bone amount triploid, reconcile system pH to 7~8 with calcium hydroxide, 2701 alkali proteases that add former dried bone amount 1 ‰ carry out the enzymolysis second time: after 2 hours, be warming up to 90 ℃ in 60 ℃ of following enzymolysis of temperature rapidly, keep high temperature 20min, make enzyme-deactivating; Carry glue 2h then under 60 ℃, the glue yield rate that obtains the enzymolysis gelatin second time after the glue drying is 17~23%, and viscosity 2.5mPas freezes power 162Bloomg.
The surplus bone water boil that doubles is only surplus a small amount of soft and do not have a bone slag of viscosity.
Embodiment 3, with the skeletal grain 10~20mm after the traditional alkali process pickling washing, the ossein 100kg of pH4~5 adds the water logging bubble 3 hours of 2 times of left and right sides volumes of ossein, adds the cathepsin of dried bone amount 1.5 ‰, is warming up to 60 ℃, carries out the enzymolysis first time; Behind the enzymolysis 3 hours, be warming up to 90 ℃ rapidly, keep high temperature 20min, make enzyme-deactivating, use pH value of solution to 6~7 behind the NaOH conditioned reaction again; Carry glue 2h then under 60 ℃, the glue yield rate that obtains the enzymolysis gelatin first time after the glue drying is 30~35%, and viscosity 2.5mPas freezes power 189Bloom g;
The water that adds 2.5 times of volumes of surplus bone amount, reconciling system pH with NaOH is 7~8, adds the trypsase of former dried bone amount 2 ‰, carries out the enzymolysis second time under 60 ℃ of temperature, enzymolysis was warming up to 90 ℃ rapidly after 2 hours, kept high temperature 20min, made enzyme-deactivating; Carry glue 2h in 60 ℃ then, obtain after the glue drying for the second time that the glue yield rate of enzymolysis gelatin is 18.5~21%, viscosity 2.7mPas freezes power 168Bloom g.
The surplus bone water boil that doubles is only surplus a small amount of soft and do not have a bone slag of viscosity.
Embodiment 4, with traditional alkali process pickling washing back skeletal grain 10~20mm, the dried ossein 100kg of pH4~5, the water logging that adds 3.5 times of ossein volumes was steeped 2.5 hours, the pepsin volume that adds dried ossein amount 2.5 ‰ is warming up to 60 ℃, carries out the enzymolysis first time, enzymolysis is warming up to 85 ℃ rapidly after 3 hours, keep high temperature 20min, make enzyme-deactivating, use pH value of solution to 6~7 behind the NaOH conditioned reaction again; Carry glue 2h in 60 ℃ then, obtain after the glue drying for the first time that the glue yield rate of enzymolysis gelatin is 30~35%, viscosity 2.5mPas freezes power 189Bloom g;
The water that adds 2.5 times of volumes of surplus bone amount, reconciling system pH with NaOH is 4~8, adds the papain of former dried bone amount 3 ‰ again, carries out the enzymolysis second time: in 55 ℃ of following enzymolysis of temperature 2 hours, be warming up to 85 ℃ rapidly, keep high temperature 20min, make enzyme-deactivating; Carry glue 2h in 60 ℃ then, obtain after the glue drying for the second time that the glue yield rate of enzymolysis gelatin is 18.9~25%, viscosity 2.2mPas freezes power 164Bloom g.
The surplus bone water boil that doubles is only surplus a small amount of soft and do not have a bone slag of viscosity.
Claims (1)
1. method that makes up preparing gelatin from enzyme degradation bone collagen comprises following processing step:
1. with the dried ossein after traditional alkali process pickling washing, steeped oil removing 2~3 hours with the water logging of 2~3 times of volumes;
2. the acid protease that adds dried ossein quality 1~3 ‰ in 55~60 ℃ of following enzyme digestion reactions 2~5 hours, is warming up under 85~100 ℃ inactivator 20~30min rapidly then; With pH value of solution to 6~7 behind the alkali conditioned reaction;
3. under 50~60 ℃ of temperature, carry glue, filter glue, dry gelatin dry;
4. in remaining ossein, add water, the bone water volume ratio was controlled at 1: 2.5~1: 3; With pH value of solution to 4~8 behind the alkali conditioned reaction; The neutrality or the slight alkaline protease that add former dried ossein quality 1~3 ‰ again in 55~60 ℃ of enzyme digestion reactions 2~3 hours, are warming up to 85~100 ℃ of following inactivator 20~30min rapidly then;
5. under 50~60 ℃ of temperature, carry glue, filter glue, dry gelatin dry;
6. remaining a small amount of ossein adds water rising temperature, boils hydrolysis.
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Cited By (11)
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CN102051130A (en) * | 2010-11-24 | 2011-05-11 | 中国科学院理化技术研究所 | Method for preparing gelatin with protease degradation ossein |
CN102732592A (en) * | 2012-07-13 | 2012-10-17 | 江南大学 | Method for preparing freshwater fish bone gelatin by enzyme process |
CN102094056B (en) * | 2009-12-14 | 2013-04-03 | 包头东宝生物技术股份有限公司 | Method for preparing soluble collagen |
CN103333939A (en) * | 2013-03-21 | 2013-10-02 | 新疆艾萨尔生物科技股份有限公司 | Method for preparing gelatin from bone collagen fibers by alkali-enzyme composite degradation |
CN103555802A (en) * | 2013-10-29 | 2014-02-05 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing gelatin by gelatin extraction through enzyme method |
CN104419742A (en) * | 2013-08-23 | 2015-03-18 | 中国科学院理化技术研究所 | Method for preparation of gelatin from bone grains as raw material |
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CN112457781A (en) * | 2020-12-19 | 2021-03-09 | 河北省微生物研究所 | Method for extracting gelatin from leather waste leather scraps by enzymolysis |
CN113016850A (en) * | 2021-04-08 | 2021-06-25 | 山东海奥斯生物科技有限公司 | Method for producing collagen casing by using pigskin |
CN115368454A (en) * | 2022-09-30 | 2022-11-22 | 斐缦(长春)医药生物科技有限责任公司 | Gelatin and preparation method thereof |
CN116694234A (en) * | 2023-06-09 | 2023-09-05 | 四川瑞宝生物科技股份有限公司 | Method for rapidly preparing bone gelatin |
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US6100381A (en) * | 1998-11-03 | 2000-08-08 | Eastman Kodak Company | Enzyme method of manufacturing gelatin |
CN1196758C (en) * | 2002-08-08 | 2005-04-13 | 中国科学院理化技术研究所 | Process for preparing gelatin from enzyme degradation bone collagen |
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CN102094056B (en) * | 2009-12-14 | 2013-04-03 | 包头东宝生物技术股份有限公司 | Method for preparing soluble collagen |
CN102051130A (en) * | 2010-11-24 | 2011-05-11 | 中国科学院理化技术研究所 | Method for preparing gelatin with protease degradation ossein |
CN102732592A (en) * | 2012-07-13 | 2012-10-17 | 江南大学 | Method for preparing freshwater fish bone gelatin by enzyme process |
CN103333939A (en) * | 2013-03-21 | 2013-10-02 | 新疆艾萨尔生物科技股份有限公司 | Method for preparing gelatin from bone collagen fibers by alkali-enzyme composite degradation |
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CN104419742A (en) * | 2013-08-23 | 2015-03-18 | 中国科学院理化技术研究所 | Method for preparation of gelatin from bone grains as raw material |
CN103555802A (en) * | 2013-10-29 | 2014-02-05 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing gelatin by gelatin extraction through enzyme method |
CN112219991A (en) * | 2019-07-15 | 2021-01-15 | 包头东宝生物技术股份有限公司 | Conditioned meat product, method for producing same and use of gelatin |
CN112457781A (en) * | 2020-12-19 | 2021-03-09 | 河北省微生物研究所 | Method for extracting gelatin from leather waste leather scraps by enzymolysis |
CN113016850A (en) * | 2021-04-08 | 2021-06-25 | 山东海奥斯生物科技有限公司 | Method for producing collagen casing by using pigskin |
CN115368454A (en) * | 2022-09-30 | 2022-11-22 | 斐缦(长春)医药生物科技有限责任公司 | Gelatin and preparation method thereof |
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 |
CN116694234A (en) * | 2023-06-09 | 2023-09-05 | 四川瑞宝生物科技股份有限公司 | Method for rapidly preparing bone gelatin |
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