CN102028711B - Enzymatically synthesized triglyceride type fish oil soft capsules and preparation method thereof - Google Patents
Enzymatically synthesized triglyceride type fish oil soft capsules and preparation method thereof Download PDFInfo
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- CN102028711B CN102028711B CN2010106072467A CN201010607246A CN102028711B CN 102028711 B CN102028711 B CN 102028711B CN 2010106072467 A CN2010106072467 A CN 2010106072467A CN 201010607246 A CN201010607246 A CN 201010607246A CN 102028711 B CN102028711 B CN 102028711B
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Abstract
The invention discloses a method for preparing enzymatically synthesized triglyceride type fish oil soft capsules. 1,000 soft capsules comprise the following raw materials by weight: 499 to 1,200g of enzymatically synthesized fish oil, 1 to 5g of natural vitamin E oil, 244g of gelatin, 100 to 220g of glycerin and 244 to 590g of distilled water. The product prepared by the method has stable quality, an acid value of less than 1, a peroxide value of less than 5 percent and an anisidine value of less than 20 percent, and can meet the requirement of food shelf life.
Description
Technical field
The present invention relates to a kind of fish oil soft capsule and preparation method thereof, particularly synthetic high concentration triglyceride type fish oil soft capsule of a kind of enzymatic and preparation method thereof.
Background technology
Be rich in the fish oil medicine of eicosapentaenoic acid (EPA) and docosahexenoic acid (DHA) synthetic, because the triglyceride type oils and fats easily is absorbed by the body and has no side effect, therefore, the triglyceride type fish oil that is combined to by ethyl ester fish oil, glycerol, lipase transesterification, in American-European pharmacopeia, be listed in the raw material for the treatment of cardiovascular and cerebrovascular disease and supplementary.Because enzymatic transesterification metallization processes is by biological respinse with the separation of ethanol in the ethyl ester fish oil out, the glycerol that is incorporated into equivalent form new with triglyceride greater than 60% the glyceride product that comprises DAG, monoglyceride, be the key that guarantees subsequent product and control diglyceride, monoglyceride content and ethyl ester in the biological respinse residual.When making soft capsule, the control ethyl ester is residual, and monoglyceride, diglyceride, content of triglyceride technical specification have become the main direction of producing qualified soft gelatin capsule.Because moisture rubber contacts with diglyceride, a sweet ester among the high concentration EPA+DHA and is very active; the capsule of preparation is because content emulsifying suction hydrolysis; cause acid value from rising to 2.5 even higher less than 1; thereby exceed the finished product acid value that requires in the quality control standard of national industry Fish oil goods and Europe, the U.S., the British Drug end product less than 1 standard, cause capsule product defective.
Summary of the invention
The purpose of this invention is to provide a kind of enzymatic synthetic glycerine three ester type fish oil soft capsules, this kind soft capsule quality is stable, and acid value is less than 1, and peroxide value is less than 5%, and anisidine value is less than 20%.
Another object of the present invention provides the preparation method of described fish oil soft capsule.
The object of the present invention is achieved like this:
A kind of enzymatic synthetic glycerine three ester type fish oil soft capsules, it is prepared from by the synthetic fish oil of enzymatic, natural complex E oil, gelatin, glycerol and distilled water, and each raw material in per 1000 soft capsules is counted by weight ratio:
Enzymatic synthesizes fish oil 499～1200g;
Natural complex E oil 1～5 g;
Gelatin 244 g;
Glycerol 100～220 g;
Surplus is distilled water.
Above-mentioned enzymatic synthetic glycerine three ester type fish oil soft capsules, each composition is in the synthetic fish oil of described enzymatic: triglyceride 60～80%, diglyceride 15～29%, monoglyceride 1.5～10%, ethyl ester 1～3.5%.
Above-mentioned enzymatic synthetic glycerine three ester type fish oil soft capsules, described gelatin are a kind of in fish glue from scale or collagen protein of fish skin glue, plant gum or the animal glue; Described plant gum is the extract of corn starch HPMC hydroxypropyl methylcellulose and pulullan polysaccharide class plant; Described animal glue is the extract in animal skins and the pig Os Bovis seu Bubali.
A kind of method for preparing above-mentioned enzymatic synthetic glycerine three ester type fish oil soft capsules, it carries out as follows:
A, colloidal sol: distilled water is put into container, and Steam Heating to 80 ℃ adds glycerol and gelatin, then after stirring deaeration, dissolving, concentrating, cross 120 order filter bags and filter, gained glue moisture Control is 40～45%, gelatin viscosity 〉=15000mpa.s, glue is 45～75 ℃ of heat preservation for standby use;
B, batching: the synthetic fish oil of enzymatic filters through 120～160 orders, adds natural complex E oil, stirs and makes its mix homogeneously, and is stand-by;
C, pelleting: control pelleting room temperature 18～26%, relative humidity 45～65%, pelleting;
D, wash ball: every pot is washed the ball time is 1.5 minutes;
E, drying: dry at twice, the drying control temperature is 25～30 ℃ for the first time, relative humidity 10～20%, dry 4～6 hours; The drying control temperature is 28～35 ℃ for the second time, relative humidity 10～20%, and dry 4～6 hours, dry rear rubber moisture Control was 8～10%;
F, pick up and look into packing, get product.
The preparation method of above-mentioned enzymatic synthetic glycerine three ester type fish oil soft capsules, described preparation technology are finished fast filling to add under the nitrogen protection condition.
The preparation method of above-mentioned enzymatic synthetic glycerine three ester type fish oil soft capsules, described natural Vitamin E oil concentration is 1000IU/g.
In the prior art of fish-oil capsule, because triglyceride, diglyceride, the imbalance of monoglyceride, can cause when making soft capsule and moisture rubber encapsulation, diglyceride, monoglyceride plays emulsification to oils and fats, and when the compacting soft gelatin capsule, a too high sweet ester, DAG can be hydrolyzed the moisture emulsifying in ethyl ester and the soft gelatin capsule coating, the content acid value is raise, its acid number is by rising to 2～3 less than 1, and As time goes on content continues hydrolysis emulsifying, and acid value continues to rise, and causes product quality to descend, so, triglyceride in the synthetic fish oil of control, diglyceride, the index of monoglyceride rationally is to make the key of qualified soft capsule.The present invention is through for many years research, draw the scientific and reasonable prescription of triglyceride, diglyceride, monoglyceride in the synthetic fish oil, can stablize the acid value index, make acid value less than 1, peroxide value less than 5%, anisidine value is less than 20%, thereby lay a good foundation for the stable capsule of preparation quality, meet American-European pharmaceutical raw material standard and the shelf-life requirement of food shelf.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
A, colloidal sol operation: get distilled water 250 g/1000 grains and put into container, use Steam Heating to 80 ℃, add glycerol 98g/1000 grain and plant gum 244 g/1000 grains, then control temperature 70 C, vacuum 0.05Mpa stirs deaeration 15 minutes; 75 ℃ of control temperature, stirring and dissolving 15 minutes; Control again 65 ℃ of temperature, vacuum 0.09Mpa, concentrated 20 minutes of deaeration; Under 55 ℃, cross the filtration of 120 order filter bags and put glue at last, gained glue moisture 40%, glue is 45 ℃ of insulations.
B, burden process: get the synthetic fish oil 510 g/1000 grains of enzymatic, its triglyceride 65%, diglyceride 28%, monoglyceride 1.5%, ethyl ester 5.5%; Filter through 120 orders, add natural complex E oil 2g/1000 grain, stirred 40 minutes, make its mix homogeneously, stand-by.
C, pelleting are qualitative: control pelleting room temperature 20%, and relative humidity 45%, content are at 500mg, and product specification is 500mg.
D, wash the ball operation: every pot is washed the ball solvent load is 5kg, and quantity is 90kg, and every pot is washed the ball time is 1.5 minutes.
E, drying process: dry at twice, the drying control temperature is 25 ℃ for the first time, relative humidity 10%, dry 5 hours.The drying control temperature is 30 ℃ for the second time, relative humidity 15%, dry 5 hours, dry rear rubber moisture 8%.
F, pick up the ball operation: choose special-shaped ball, large piller, bubble ball, heterochromatic ball, leakage of oil ball.
G, packing, warehouse-in: carry out exterior and interior packing, pick test is qualified, warehouse-in.
Embodiment 2:
A, colloidal sol operation: get distilled water 400 g/1000 grains and put into container, use Steam Heating to 80 ℃, add glycerol 150g/1000 grain and animal glue 244g/1000 grain, then control 80 ℃ of temperature, vacuum 0.05Mpa stirs deaeration 25 minutes; 80 ℃ of control temperature, stirring and dissolving 20 minutes; Control again 75 ℃ of temperature, vacuum 0.09Mpa, concentrated 25 minutes of deaeration; Under 70 ℃, cross the filtration of 120 order filter bags and put glue at last, gained glue moisture 40%, glue is 45 ℃ of insulations.
B, burden process: get the synthetic fish oil 700 g/1000 grains of enzymatic, its triglyceride 75%, diglyceride 19%, monoglyceride 1.5%, ethyl ester 6%; Filter through 120 orders, add natural complex E oil 4g/1000 grain, stirred 50 minutes, make its mix homogeneously, stand-by.
C, pelleting are qualitative: control pelleting room temperature 20%, and relative humidity 45%, content are at 500mg, and product specification is 500mg.
D, wash the ball operation: every pot is washed the ball solvent load is 5kg, and quantity is 90kg, and every pot is washed the ball time is 1.5 minutes.
E, drying process: dry at twice, the drying control temperature is 25 ℃ for the first time, relative humidity 10%, dry 5 hours; The drying control temperature is 30 ℃ for the second time, relative humidity 15%, dry 5 hours, dry rear rubber moisture 8.5%.
F, pick up the ball operation: choose special-shaped ball, large piller, bubble ball, heterochromatic ball, leakage of oil ball.
G, packing, warehouse-in: carry out exterior and interior packing, pick test is qualified, warehouse-in.
Embodiment 3:
A, colloidal sol operation: get distilled water 580 g/1000 grains and put into container, use Steam Heating to 80 ℃, add glycerol 200g/1000 grain and collagen protein glue 244 g/1000 grains, then control 80 ℃ of temperature, vacuum 0.05Mpa stirs deaeration 30 minutes; 85 ℃ of control temperature, stirring and dissolving 30 minutes; Control again 80 ℃ of temperature, vacuum 0.09Mpa, concentrated 30 minutes of deaeration; Under 80 ℃, cross the filtration of 120 order filter bags and put glue at last, gained glue moisture 40%, glue is 45 ℃ of insulations.
B, burden process: get the synthetic fish oil 510 g/1000 grains of enzymatic, its triglyceride 80%, diglyceride 15%, monoglyceride 2.5%, ethyl ester 2.5%; Filter through 120 orders, add natural complex E oil 5g/1000 grain, stirred 70 minutes, make its mix homogeneously, stand-by.
C, pelleting are qualitative: control pelleting room temperature 20%, and relative humidity 45%, content are at 500mg, and product specification is 500mg.
D, wash the ball operation: every pot is washed the ball solvent load is 5kg, and quantity is 90kg, and every pot is washed the ball time is 1.5 minutes.
E, drying process: dry at twice, the drying control temperature is 30 ℃ for the first time, relative humidity 20%, dry 6 hours; The drying control temperature is 35 ℃ for the second time, relative humidity 10%, dry 6 hours, dry rear rubber moisture 9%.
F, pick up the ball operation: choose special-shaped ball, large piller, bubble ball, heterochromatic ball, leakage of oil ball.
G, packing warehouse-in: carry out exterior and interior packing, pick test is qualified, warehouse-in.
Claims (4)
1. enzymatic synthetic glycerine three ester type fish oil soft capsules is characterized in that, it is prepared from by the synthetic fish oil of enzymatic, natural complex E oil, gelatin, glycerol and distilled water, and each raw material in per 1000 soft capsules is counted by weight ratio:
Enzymatic synthesizes fish oil 499～1200g;
Natural complex E oil 1～5 g;
Gelatin 244 g;
Glycerol 100～220 g;
Surplus is distilled water;
Each composition is in the synthetic fish oil of described enzymatic: triglyceride 60～80%, diglyceride 15～29%, monoglyceride 1.5～10%, ethyl ester 1～3.5%.
2. enzymatic synthetic glycerine three ester type fish oil soft capsules according to claim 1 is characterized in that, described gelatin is a kind of in fish glue from scale or collagen protein of fish skin glue, plant gum or the animal glue; Described plant gum is the extract of corn starch HPMC hydroxypropyl methylcellulose and pulullan polysaccharide class plant; Described animal glue is the extract in animal skins and the pig Os Bovis seu Bubali.
3. one kind prepares the as claimed in claim 1 or 2 method of enzymatic synthetic glycerine three ester type fish oil soft capsules, it is characterized in that, it carries out as follows:
A, colloidal sol: distilled water is put into container, Steam Heating to 80 ℃, add glycerol and gelatin, then after stirring deaeration, dissolving, concentrating, cross 120 order filter bags and filter, add gelatin, gained glue moisture Control is 40～45%, gelatin viscosity 〉=15000mpa.s, glue is 45～75 ℃ of heat preservation for standby use;
B, batching: the synthetic fish oil of enzymatic filters through 120～160 orders, adds natural complex E oil, stirs and makes its mix homogeneously, and is stand-by;
C,Pelleting: control pelleting room temperature 18～26%, relative humidity 45～65%, pelleting;
D, wash ball: every pot is washed the ball time is 1.5 minutes;
E, drying: dry at twice, the drying control temperature is 25～30 ℃ for the first time, relative humidity 10～20%, dry 4～6 hours; The drying control temperature is 28～35 ℃ for the second time, relative humidity 10～20%, and dry 4～6 hours, dry rear rubber moisture Control was 8～10%;
F, pick up and look into packing, get product.
4. the method for preparing enzymatic synthetic glycerine three ester type fish oil soft capsules according to claim 3 is characterized in that, described preparation technology finishes fast filling to add under the nitrogen protection condition.
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| CN103349289A (en) * | 2013-06-14 | 2013-10-16 | 芜湖市诺康生物科技有限公司 | Preparation method of fish oil soft capsules |
| CN105566103B (en) | 2014-10-13 | 2019-02-19 | 浙江医药股份有限公司新昌制药厂 | A kind of preparation method of glycerol ester type polyunsaturated fatty acid |
| CN104705772B (en) * | 2015-01-28 | 2016-09-14 | 汤臣倍健股份有限公司 | A kind of production technology improving soft capsule leakage of oil |
| CN105311072A (en) * | 2015-08-25 | 2016-02-10 | 北京世纪合辉医药科技股份有限公司 | Healthcare product capable of improving memory and production method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101112405A (en) * | 2007-08-10 | 2008-01-30 | 姚广滨 | Drug for curing coronary disease and method for preparing the same |
| CN101427816A (en) * | 2008-11-25 | 2009-05-13 | 许震 | Fishy smell removed polydiluted acid capsule |
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| CN101161819A (en) * | 2007-10-12 | 2008-04-16 | 广东海洋大学 | Method for preparing n-3PUFA ocean glycerin ester by enzymatical process |
| CN101736044B (en) * | 2008-11-18 | 2013-10-23 | 浙江海洋学院 | Method for continuous enzymatic synthesis of n-3PUFA glyceride |
| CN101818176B (en) * | 2010-04-09 | 2013-05-15 | 浙江兴业集团有限公司 | Method for transforming fatty acid ethyl ester into glyceride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101112405A (en) * | 2007-08-10 | 2008-01-30 | 姚广滨 | Drug for curing coronary disease and method for preparing the same |
| CN101427816A (en) * | 2008-11-25 | 2009-05-13 | 许震 | Fishy smell removed polydiluted acid capsule |
Non-Patent Citations (1)
| Title |
|---|
| 宁正祥，彭凯文，汤毅珊，谭龙飞，谭兴和.鱼油多不饱和脂酰甘油酯的非水相酶促合成及溶剂分子性质的影响.《食品科学》.1995,第16卷(第5期), * |
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