CN103652366B - A kind of stabilization micro-capsule coating Mercaptamine and preparation method thereof - Google Patents
A kind of stabilization micro-capsule coating Mercaptamine and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of stabilization micro-capsule coating Mercaptamine and preparation method thereof, it is mainly made up of the following raw material of quality proportioning：20 ~ 55 parts of Mercaptamine, 15 ~ 35 parts of cornstarch, 0.1 ~ 10 part of sodium carboxymethylcellulose, 1 ~ 10 part of sodium alginate, 0.1 ~ 10 part of ethyl cellulose, 10 ~ 15 parts of beta cyclodextrin, 10 ~ 50 parts of Brazil wax.The invention provides a kind of stabilization micro-capsule coating Mercaptamine and its preparation technology, the Mercaptamine easily oxidized, deficiency of the easy moisture absorption is efficiently solved, so as to reach the purpose of protection Mercaptamine；Meanwhile, farthest limit Mercaptamine and discharge under one's belt, it is to avoid the generation of gastric ulcer, and fully discharged in enteron aisle, so as to more effectively by animal use, promote growth of animal, with preferable application prospect.
Description
（One）Technical field
The present invention relates to a kind of stabilization micro-capsule coating Mercaptamine and preparation method thereof.
（Two）Background technology
Mercaptamine（Cysteamine, CS）It is the part of acetyl coenzyme A, because of it also known as Mercamine Cysteamine
There are various biological functions containing active sulfydryl and amino, be the bioactivator in animal body.Many studies have shown that,
CS is the concentration by reducing SS in body, weakens or eliminates SS and growth-promoting effect is reached to the inhibitory action of digestive system；
SS Endocrine systems are more importantly released, especially to the inhibitory action of GH, IGF-1, adds the secretion of GH, IGF-1 etc.
By force, promote growth of animal, improve feedstuff-meat ratio.
Cysteamine is white crystals, there is foreign odor, and soluble in water and alcohol is reacted to disulphide in atmosphere.By
In the unstable characteristic of its free base, hydrochloride C is made generally in2H7NSHCl, need to keep in dark place.But Mercaptamine
The moisture absorption is easily aoxidized, causes it to be oxidized quickly in processing and storage, so as to influence the using effect of product.In addition,
Because Mercaptamine is easily oxidized to disulphide in atmosphere, coat of the stomach can be stimulated under one's belt, produce serious gastric ulcer, because
This may not apply to large-scale production.
Currently for these shortcomings of Mercaptamine, in the market is also occurred in that by the Mercaptamine of coating,
Some Mercaptamines are only simple mixing granulation, and the effect of coating is not reached；Though some Mercaptamines
So by coating, but whether whether it stablizes during storage, stablize when particularly mixing with reproducibility raw material, in animal intestine
Whether stomach can be crossed in road, reach slow release effect, need further research.
（Three）The content of the invention
It is an object of the invention to provide a kind of stabilization micro-capsule coating Mercaptamine and its preparation technology, make cysteamine salt
Hydrochlorate can keep stabilization in natural environment, and redox is not susceptible to when mixing and coexist with the reproducibility raw material such as sodium selenite
Reaction inactivation discoloration, it is to avoid Mercaptamine is oxidized during processing and storage.
The technical solution adopted by the present invention is：
A kind of stabilization micro-capsule coating Mercaptamine, is mainly made up of the following raw material of quality proportioning：Cysteamine hydrochloric acid
20~55 parts of salt, 15~35 parts of cornstarch, 0.1~10 part of sodium carboxymethylcellulose, 1~10 part of sodium alginate, ethyl cellulose
0.1~10 part of element, 10~15 parts of beta-schardinger dextrin, 10~50 parts of Brazil wax.It is above-mentioned to prepare the stabilization micro-capsule coating half
The primary raw material of cystamine hydrochloride, not including solvent used in preparation process, such as water and ethanol.
Preferably, its primary raw material quality proportioning is as follows：28~35 parts of Mercaptamine, 20~35 parts of cornstarch,
1~5 part of sodium carboxymethylcellulose, 1~5 part of sodium alginate, 1~5 part of ethyl cellulose, 10~15 parts of beta-schardinger dextrin, cohune
20~30 parts of palmitic acid wax.
The invention further relates to the preparation method of the stabilization micro-capsule coating Mercaptamine, methods described includes：
（1）The Mercaptamine of formula ratio is put into 75~90 DEG C of heating fusings in a kettle.；
（2）The sodium carboxymethylcellulose of formula ratio is configured to the carboxymethylcellulose calcium of mass concentration 1~10% with distilled water
Sodium water solution；
（3）By the cornstarch of formula ratio, sodium alginate, ethyl cellulose and beta-schardinger dextrin put into step（2）Prepare
Sodium carboxymethyl cellulose solution in, stirring mixing, 100~200r/min of rotating speed, 15~30min of time；
（4）The Mercaptamine that will be melted adds step（3）In the mixture of preparation, mix, then the granulation of 20 mesh, puts
In cyclone fluidized bed drying, 60~80 DEG C of EAT, 35~55 DEG C of leaving air temp；
（5）Will appropriate 95% food-grade ethanol add reactor in be heated to 55~75 DEG C, then by the babassu of formula ratio
Wax dissolves in adding ethanol；
（6）With the Brazil wax of dissolving to step（4）Obtained particle bottom spray is coated, 0.2~0.3Mpa of atomizing pressure,
Wriggling 100~200r/min of flow rate pump, sieving（10~20 mesh）, obtain the stabilization micro-capsule coating Mercaptamine.
Preferably, its primary raw material quality proportioning is as follows in preparation process：28~35 parts of Mercaptamine, cornstarch
20~35 parts, 1~5 part of sodium carboxymethylcellulose, 1~5 part of sodium alginate, 1~5 part of ethyl cellulose, beta-schardinger dextrin 10~15
Part, 20~30 parts of Brazil wax, 95% food-grade ethanol quality are 1~5 times of Brazil wax quality.
The present invention is improved to existing coating process, and Mercaptamine is solved easily and selenous acid by physics mode
The shortcoming that the reproducibility such as sodium raw material occurs redox reaction inactivation and changes colour, has good stability in process；Its
When being used as feed addictive, the shelf-life of feed can be extended, and other nutritional ingredients do not destroyed in feed, can quilt
Animal fully absorbs utilization；Detected by simulating animal gastric juice method, the retention rate after its 2h in gastric juice is 96.4%, in machine
Stabilization is kept in body stomach, is detected by simulating animal intestinal juice method, dissolution rates of its 8h in intestinal juice is 92.5%, in body intestines
Slowly discharged in road, can reach and wrap to live the molten good coating effect for drawing.
The beneficial effects are mainly as follows：The invention provides it is a kind of stabilization micro-capsule coating Mercaptamine and
Its preparation technology, efficiently solves the Mercaptamine easily oxidized, deficiency of the easy moisture absorption, so as to reach protection cysteamine hydrochloric acid
The purpose of salt；Meanwhile, farthest limit Mercaptamine and discharge under one's belt, it is to avoid the generation of gastric ulcer, and in intestines
Fully discharged in road, so as to more effectively by animal use, promote growth of animal, with preferable application prospect.
（Four）Brief description of the drawings
Fig. 1 mixes for micro-capsule coating Mercaptamine product of the present invention and other coated products with sodium selenite simultaneously after
Photo；
Fig. 2 is dissolution rate testing result of the micro-capsule coating Mercaptamine of the present invention in gastric juice；
Fig. 3 is dissolution rate testing result of the micro-capsule coating Mercaptamine of the present invention in intestinal juice.
（Five）Specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1：
（1）Weigh each raw material：Mercaptamine 28kg, cornstarch 33.5kg, sodium carboxymethylcellulose 1.5kg, sea
Mosanom 1kg, ethyl cellulose 1kg, beta-schardinger dextrin 10kg, Brazil wax 25kg and 95% food-grade ethanol 40kg.
（2）Preparation method：The first step, 80~85 DEG C of heating fusings in a kettle. are put by Mercaptamine；Second step,
Sodium carboxymethylcellulose is configured to 5% with distilled water（w/w）Sodium carboxymethyl cellulose solution；3rd step, by cornstarch,
Sodium alginate, ethyl cellulose and beta-schardinger dextrin, put into the sodium carboxymethyl cellulose solution of second step preparation, and stirring is mixed
Close, rotating speed 150r/min, time 20min；4th step, the Mercaptamine that will be melted adds mixture prepared by the 3rd step
In, mix, then the granulation of 20 mesh, is placed in cyclone fluidized bed drying, 60~80 DEG C of EAT, 35~55 DEG C of leaving air temp；The
Five steps, heat 60~70 DEG C, then will be dissolved in Brazil wax addition hot ethanol during food-grade ethanol is added into reactor；6th
Step, is sprayed to particle bottom obtained in the 4th step with the Brazil wax of dissolving and is coated, 0.2~0.3Mpa of atomizing pressure, peristaltic pump stream
100~200r/min of speed, crosses 12 mesh sieves, final to obtain 12~40 mesh products.
（3）The micro-capsule coating Mercaptamine of gained, with preferable mobility, and easily mixes with all feeds.
Sample bag hermetic package, is stored at shady and cool ventilation, stores 1 year, and its proterties is constant, with good stability, meets feed
The requirement of additive.
Embodiment 2：
（1）Weigh each raw material：Mercaptamine 30kg, cornstarch 23kg, sodium carboxymethylcellulose 3kg, alginic acid
Sodium 2kg, ethyl cellulose 2kg, beta-schardinger dextrin 10kg, Brazil wax 30kg and 95% food-grade ethanol 45kg.
（2）Preparation method：The first step, 80~85 DEG C of heating fusings in a kettle. are put by Mercaptamine；Second step,
Sodium carboxymethylcellulose is configured to 10% sodium carboxymethyl cellulose solution with distilled water；3rd step, by cornstarch, marine alga
Sour sodium, ethyl cellulose and beta-schardinger dextrin, put into the sodium carboxymethyl cellulose solution of second step preparation, and stirring mixes,
Rotating speed 120r/min, time 20min；4th step, the Mercaptamine that will be melted is added in mixture prepared by the 3rd step, is mixed
It is even, 20 mesh granulations are carried out, it is placed in cyclone fluidized bed drying, 60~80 DEG C of EAT, 35~55 DEG C of leaving air temp；5th step,
60~70 DEG C are heated during food-grade ethanol is added into reactor, then will be dissolved in Brazil wax addition hot ethanol；6th step, uses
The Brazil wax of dissolving is coated to particle bottom spray obtained in the 4th step, 0.2~0.3Mpa of atomizing pressure, wriggling flow rate pump 100
~200r/min, crosses 12 mesh sieves, final to obtain 12~40 mesh products.
（3）Gained micro-capsule coating Mercaptamine product and other coated products mix with sodium selenite simultaneously after, institute
Micro-capsule coating Mercaptamine product nondiscolouring is obtained, and becomes red or yellow after the mixing of other coated products（Referring to Fig. 1）,
Therefore product of the present invention has good stability in process.
（4）The micro-capsule coating Mercaptamine of gained, with preferable mobility, and easily mixes with all feeds.
Sample bag hermetic package, is stored at shady and cool ventilation, stores 1 year, and its proterties is constant, with good stability, meets feed
The requirement of additive.
（5）Micro-capsule coating Mercaptamine dissolution determination
1. the measure of micro-capsule coating Mercaptamine dissolution rate in gastric juice：Weigh（2）The finished product 2g of preparation, is placed in
In stripping rotor, plus simulated gastric fluid 400ml, 100r/min rotating speed, 38 DEG C of temperature.Fixed point（0.5h, 1.0h, 1.5h and 2.0h）Take
Sample, filtering, precision measures 5ml filtrates, is diluted with water to 10ml, shakes up rear mocromembrane filtering, and upper machine is determined.Dissolution rate computing formula
It is as follows：
In formula：
A1--- the area of Mercaptamine chromatographic peak in sample chromatogram figure；
C1--- the concentration of standard sample, unit is mg/ml；
A2--- the chromatographic peak area of Mercaptamine control；
M1--- the quality of Mercaptamine sample, unit is mg；
800 --- Sample Dilution multiple
Result is shown in Fig. 2, and as seen from the figure, micro-capsule coating Mercaptamine stabilization in gastric juice, dissolution rate is very low, by 2h
Afterwards, dissolution rate is only 3.6%.
2. the measure of micro-capsule coating Mercaptamine dissolution rate in intestinal juice：By the above-mentioned sample for finishing gastric juice dissolution rate
Filtered, and rinsed in neutrality with water, be placed in stripping rotor, plus simulated intestinal fluid 400ml, 100r/min rotating speed, temperature 38
℃.Fixed point（2h, 4h, 6h and 8h）Sampling, filtering, precision measures 5ml filtrates, is diluted with water to 10ml, and mocromembrane filtering, upper machine is surveyed
It is fixed.Dissolution rate computing formula is as follows：
In formula：
A1--- the area of Mercaptamine chromatographic peak in sample chromatogram figure；
C1--- the concentration of standard sample, unit is mg/ml；
A2--- the chromatographic peak area of Mercaptamine control；
M1--- the quality of Mercaptamine sample, unit is mg；
800 --- Sample Dilution multiple
Result is shown in Fig. 3, and as seen from the figure, micro-capsule coating Mercaptamine slowly discharges in intestinal juice, by 8h, dissolution rate
Reach 92.5%.
From result above, product of the present invention has reached and has wrapped to live the molten coating effect for drawing.
（7）Product of the present invention uses the front and rear contrast with the existing coating Mercaptamine product of Isodose
160 body conditions of selection are good, average weight is the DLY tri-crossbreeding of 60kg, are randomly divided into two groups, every group
Four repetitions, each repeats 10 pigs（Male and female half and half）.Four groups of test groups feed containing 0,200g/t micro-capsule coatings of the present invention respectively
The daily ration of Mercaptamine.Test pig group feeding powder, free choice feeding and drinking-water, carry out routine immunization program, and feeding and management is pressed
Routine is carried out.Pig house is carried out disinfection before experiment.5 days preliminary trial periods, positive 40 days phases of examination.Daily record food consumption during experiment
Amount.After off-test, stop being weighed after raising 24h, calculate the lean meat percentage of test group（%）, the thickness of backfat（CM）, eye muscle area（CM2）、
Hunter L, Hunter a and Hunter b, as a result see the table below：
| Inspection target | Control group | Test group |
| Lean meat percentage（%） | 67.57 | 71.71 |
| The thickness of backfat（CM） | 3.00 | 2.70 |
| Eye muscle area（CM2） | 49.10 | 51.10 |
| Hunter L | 43.81 | 46.87 |
| Hunter a | 7.45 | 7.47 |
| Hunter b | 10.7 | 9.66 |
Analysis record data, test group improves 6.1% than control group lean meat percentage, and the thickness of backfat reduces 0.3cm, eye muscle face
Product increased 4.1%.
Result shows that growing and fattening pigs are remarkably improved the lean meat of fattening pig using micro-capsule coating Mercaptamine of the invention
Rate and eye muscle area, reduce the thickness of backfat, improve meat yellowish pink, and then improve carcass quality, and test group pig is eaten for a long time this
The coating Mercaptamine of invention, does not have negative effect to feed intake, does not occur the situation that pig suffers from gastrointestinal disease yet and goes out
It is existing, it is seen that coating Mercaptamine long-term consumption security of the invention is stronger.
Claims (3)
1. a kind of preparation method of stabilization micro-capsule coating Mercaptamine, it is characterised in that methods described includes：
(1) Mercaptamine of formula ratio is put into 75~90 DEG C of heating fusings in a kettle.；
(2) sodium carboxymethylcellulose of formula ratio is configured to the sodium carboxymethylcellulose of mass concentration 1~10% with distilled water
The aqueous solution；(3) by the cornstarch of formula ratio, sodium alginate, ethyl cellulose and beta-schardinger dextrin put into step (2) preparation
Sodium carboxymethyl cellulose solution in, stirring mixing, 100~200r/min of rotating speed, 15~30min of time；
(4) during the Mercaptamine that will be melted adds mixture prepared by step (3), mix, then the granulation of 20 mesh, is placed in rotation
Stream fluidized bed drying, 60~80 DEG C of EAT, 35~55 DEG C of leaving air temp；
(5) will appropriate 95% food-grade ethanol add reactor in be heated to 55~75 DEG C, then by the Brazil wax of formula ratio
Add dissolving in ethanol；
(6) particle bottom obtained in step (4) is sprayed with the Brazil wax of dissolving and is coated, 0.2~0.3Mpa of atomizing pressure is wriggled
100~200r/min of flow rate pump, sieving obtains the stabilization micro-capsule coating Mercaptamine；
The proportioning of the raw material is as follows：20~55 parts of Mercaptamine, 15~35 parts of cornstarch, sodium carboxymethylcellulose
0.1~10 part, 1~10 part of sodium alginate, 0.1~10 part of ethyl cellulose, 10~15 parts of beta-schardinger dextrin, Brazil wax 10~
50 parts.
2. the method for claim 1, it is characterised in that its primary raw material quality proportioning is as follows：Mercaptamine 28~
35 parts, 20~35 parts of cornstarch, 1~5 part of sodium carboxymethylcellulose, 1~5 part of sodium alginate, 1~5 part of ethyl cellulose, β-
10~15 parts of cyclodextrin, 20~30 parts of Brazil wax, 95% food-grade ethanol quality are 1~5 times of Brazil wax quality.
3. the stable micro-capsule coating Mercaptamine that method as claimed in claim 1 or 2 is prepared.
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| EP3308773A1 (en) | 2016-10-11 | 2018-04-18 | Recordati Industria Chimica E Farmaceutica SPA | Formulations of cysteamine and cysteamine derivatives |
| CN108740371B (en) * | 2018-04-04 | 2021-07-30 | 广州智特奇生物科技股份有限公司 | Enteric coating material, zinc oxide coated by coating material and preparation method thereof |
| CN109717481B (en) * | 2018-12-27 | 2022-04-26 | 广州智特奇生物科技股份有限公司 | Preparation process of coated probiotics |
| CN115918785A (en) * | 2022-12-25 | 2023-04-07 | 杭州康德权饲料有限公司 | Application of cysteamine or its salt in preparing feed additive for preventing and treating proventriculitis and myogastritis of poultry |
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| CN1666631A (en) * | 2005-04-09 | 2005-09-14 | 李浙烽 | Slow releasing integument composition of cysteamine or its salts, processing technique and application thereof |
| CN101513226B (en) * | 2009-03-12 | 2012-08-08 | 广州智特奇生物科技有限公司 | Microcapsule of phytase and preparation method thereof |
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