CN101703472A - Granulating coated slow release product of cysteamine hydrochloride and preparation method thereof - Google Patents
Granulating coated slow release product of cysteamine hydrochloride and preparation method thereof Download PDFInfo
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- CN101703472A CN101703472A CN200910198570A CN200910198570A CN101703472A CN 101703472 A CN101703472 A CN 101703472A CN 200910198570 A CN200910198570 A CN 200910198570A CN 200910198570 A CN200910198570 A CN 200910198570A CN 101703472 A CN101703472 A CN 101703472A
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Abstract
The invention discloses a granulating coated slow release product of cysteamine hydrochloride and a preparation method thereof. The product is obtained by taking cysteamine hydrochloride, corn starch, vitamin C, powdered glucose, stearic acid and 85wt percent phosphoric acid solution as raw materials through the processes of heating for dissolving, millard reaction, stabilization treatment, atomized granulation, hardening waterproof coating, enteric coating, drying, sieving and the like, wherein the content of the cysteamine hydrochloride in the product is more than or equal to 30.50 percent and the water content ranges from 0 percent to 8.0 percent. The method thoroughly eradicates the odor of the cysteamine hydrochloride, the product has the fragrance of bulked corn, and the glucose added in the millard reaction can conduct physical coverage and cause the cysteamine hydrochloride to be slowly released, thus increasing the palatability of products. The addition of glucose in full-price materials not only does not affect feed intake, but also can increase the feed intake. In the process of technological treatment and storage of the products, the content of cysteamine hydrochloride is stable.
Description
Technical field
The present invention relates to Mercaptamine, be specifically related to a kind of granulating coated slow release product of cysteamine hydrochloride and preparation method thereof.
Background technology
Mercaptamine can suppress the secretion of animal body somatostatin, promotes growth of animal, improves feedstuff-meat ratio and proteinic deposition.At present, the Mercaptamine product mainly contains powder-type and granular pattern product.
Because Mercaptamine itself has very strong stink abnormal smells from the patient and bitterness mouthfeel, therefore animal feed intake is had a significant impact.Simultaneously, the very easily oxidation moisture absorption of Mercaptamine, cause finished product granulate, art for coating is handled and the product put procedure in, the very fast oxidation of Mercaptamine influences the result of use of product.At present, the technical matters that Mercaptamine product on the market adopts is that the physics method is granulated and coating, because slow-release material and coating ratio are lower, so palatability and stability problem exist simultaneously.
Summary of the invention
Technical problem to be solved by this invention provides a kind of granulating coated slow release product of cysteamine hydrochloride and preparation method thereof, use product that this method makes and both removed the stink of Mercaptamine, the slow suitable effect of Mercaptamine is covered and strengthened to physics again, increased palatability; Stability improves in PROCESS FOR TREATMENT and the storage, has guaranteed that the product nucleus does not lose, for the product result of use provides stable technical guarantee.
For reaching above purpose, the present invention realizes by the following technical solutions:
A kind of granulating coated slow release product of cysteamine hydrochloride by mass percentage, comprises following component:
Mercaptamine 31.5～35.6%
Corn starch 30.5～35.5%
Vitamin C 0.7～1.5%
Glucose powder 25.0～30.5%
Stearic acid 5.0～10.0%
85wt% phosphoric acid 2.0～4.0%.
Mercaptamine content 〉=30.50wt% in the described slow release product, moisture 0-8.0wt%.
The preparation method of described granulating coated slow release product of cysteamine hydrochloride may further comprise the steps:
(1) Mercaptamine fusing: Mercaptamine, vitamin C are pressed above-mentioned quality proportioning splendid attire in plastic containers, and the boiling water bath heating is stirred to fully and dissolves, and is heated to 80-85 ℃.
(2) add glucose powder and fusing: when the Mercaptamine melt reaches 70-80 ℃, add glucose powder, heated and stirred continues to be heated to 90-95 ℃ to dissolving fully.
(3) Maillard reaction: when above-mentioned melt is heated to 90-95 ℃, heat while stirring in boiling water bath, carry out Maillard reaction, reaction 85-100min forms Maillard reaction liquid.
(4) cool off, add the 85wt% phosphoric acid solution: take out the Maillard reaction liquid container in the boiling water bath, put into psychrolusia, continue to stir, be cooled to 50-60 ℃, add the 85wt% phosphoric acid solution while stirring, stir.
(5) granulate: drop into corn starch in cyclone fluidized bed, the Maillard reaction liquid that adds the 85wt% phosphoric acid solution is continuing under the stirring, and spraying enters in the corn starch material bed granulates.
(6) granule sclerosis, waterproof coating: after granulation is finished, dry 20-30min, 90-100 ℃ of atomizing stearic acid melt carries out waterproof coating and granule sclerosis to granule.
(7) granule enteric coating: after the stearic acid coating was finished, atomizing polypropylene acid resin ethanol coating solution carried out enteric coating to granule.Used coating solution is the alcoholic solution of polyacrylic resin II and polyacrylic resin III.
(8) cooling packing: after treating the dry 20-30min of above-mentioned granule materials, shut down, take out material, packing is cooled to 40-45 ℃, crosses 10 mesh standard sieves, and metering packing gets finished product.
Described glucose and Mercaptamine are removed the stink and the bitterness of Mercaptamine itself through Maillard reaction under acid condition.
Mercaptamine in the coated slow release product of the present invention adopts following detection method:
1.1 measuring principle
With the starch solution is indicator, with standard iodine solution oxide titration Mercaptamine solution.
1.2 reagent solution and equipment
(1) 0.1mol/L iodine standard solution
(2) 6.0mol/L glacial acetic acid solution
Accurately measure glacial acetic acid solution 350ml, be diluted to 1000ml with deionized water.
(3) 0.5wt% starch indicator
Take by weighing 1.0 gram starch, add the 5ml deionized water, stir into pasty state, under stirring pastel is joined in the ebullient water of 190ml, boil 1～2min, after the cooling, be diluted to 200ml with deionized water, the operating period was two weeks.
(4) equipment
Sensibility reciprocal 0.0001 gram analytical balance, 50ml acid buret, constant temperature oven.
1.3 assay method
Take by weighing testing sample 0.2 gram (accurately to 0.0002 gram) in the tool plug triangular flask of 150ml dried and clean, glacial acetic acid solution 15ml dissolving with 6.0mol/L, the 50ml deionized water reinjects, cover stopper, the 120r/min 20min that vibrates makes the abundant stripping of Mercaptamine, adds 0.5% starch indicator 1.0ml, is terminal point with the iodine standard solution titration to just showing blueness, does blank simultaneously.
1.4 the result calculates
In the formula:
C is the concentration (mol/L) of iodine standard solution.
V
1Volume (ml) for sample quota of expenditure solution.
V
2Volume (ml) for blank quota of expenditure solution.
G is the quality (gram) of sample.
113.6 be the molecular weight of half Guang hydrochlorate.
The granulating coated slow release product of cysteamine hydrochloride that the present invention adopts Maillard reaction to make, thoroughly removed the stink of Mercaptamine, make stink be transformed into the fragrance of popcorn, the glucose at high proportion that adds in the Maillard reaction, the slow suitable effect of Mercaptamine is covered and strengthened to energy physics, increase palatability, the phosphoric acid solution of the 85wt% that adds in the preparation process, Mercaptamine is under the weak acid microenvironment, be not easy oxidation, increased the stability in PROCESS FOR TREATMENT and the storage, guaranteed that the product nucleus does not lose, for the product result of use provides stable technical guarantee.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further described, but does not limit the present invention:
Embodiment 1
One, prescription:
50 kilograms of Mercaptamines;
50 kilograms of corn starchs
1.5 kilograms of vitamin Cs;
40 kilograms of glucose powders;
10 kilograms of stearic acid;
85wt% phosphatase 24 .0 kilogram;
Above-mentioned raw materials all can be buied in raw materials market.
Two, the operating procedure step is as follows:
(1) Mercaptamine fusing: Mercaptamine, vitamin C splendid attire are in plastic containers, and boiling water bath is heated to fully and dissolves, and are heated to 80 ℃.
(2) add glucose powder, fusing: when the melt temperature reaches 80 ℃, add the food stage glucose powder, heat and be stirred to fully and dissolve, and be heated to 90 ℃.
(3) Maillard reaction: when the melt temperature reaches 90 ℃, in boiling water bath, heat while stirring, carry out Maillard reaction, response time 85min.
(4) cool off, add the 85wt% phosphoric acid solution: take out the plastics reaction vessel in the boiling water bath, put into lasting stirring of psychrolusia and be cooled to 60 ℃, add the 85wt% phosphoric acid solution while stirring, stir, guarantee that phosphoric acid is evenly distributed in the solution.
(5) granulate: drop into corn starch in cyclone fluidized bed, the Maillard reaction liquid that adds the 85wt% phosphoric acid solution is being continued under the stirring, spraying enters in the corn starch material bed granulates.
(6) granule sclerosis, waterproof coating: granulate finish after, dry 25min sprays into atomize heat fused, temperature and is 90 ℃ stearic acid melt, and granule is carried out the waterproof coating, plays the granule induration simultaneously.
(7) granule enteric coating: after the stearic acid coating was finished, preparation coating solution sprayed into atomizing polyacrylic resin alcoholic solution, and granule is carried out enteric coating.
The alcoholic solution compound method of polyacrylic resin II and polyacrylic resin III is as follows: accurate weighing 2 kilograms of polyacrylic resin II granule and 2 kilograms of polyacrylic resin III granules; Above-mentioned 4 kilograms of resin particles of accurate weighing are added in 24 kilograms of 95v/v% alcoholic solutions, stir, be dissolved to clarification fully.
(8) drying: dry materials 25min.
(9) cooling, packing: shut down, take out material, packing is cooled to 40 ℃ of temperature, crosses 10 mesh standard sieves, and metering packing gets finished product.
Three, Mercaptamine content detection:
Measure according to aforementioned cysteamine detection method of content, getting Mercaptamine content is 32.28wt%, and moisture is 5.13%.Follow the tracks of after 5 months, measuring Mercaptamine content is 32.05wt%, and moisture is 5.38%.
This product is faint yellow, has popcorn fragrance, graininess, and free-running property is good.
Embodiment 2
One, prescription:
52 kilograms of Mercaptamines;
50 kilograms of corn starchs
1.25 kilograms of vitamin Cs;
42 kilograms of glucoses;
8 kilograms of stearic acid;
85wt% phosphatase 24 .25 kilogram;
Above-mentioned raw materials all can be buied in raw materials market.
Two, the operating procedure step is as follows:
(1) Mercaptamine fusing: Mercaptamine, vitamin C splendid attire are in plastic containers, and boiling water bath is heated to fully and dissolves, and are heated to 85 ℃.
(2) add glucose powder, fusing: when the melt temperature reaches 85 ℃, add the food stage glucose powder, heat and be stirred to fully and dissolve, and be heated to 95 ℃.
(3) Maillard reaction: when the melt temperature reaches 95 ℃, in boiling water bath, heat while stirring, carry out Maillard reaction, response time 100min.
(4) cooling adds the 85wt% phosphoric acid solution: take out the plastics reaction vessel in the boiling water bath, put into lasting stirring of psychrolusia and be cooled to 55 ℃, add the 85wt% phosphoric acid solution while stirring, stir, guarantee that phosphoric acid is evenly distributed in the solution.
(5) granulate: drop into corn starch in cyclone fluidized bed, the Maillard reaction liquid that adds the 85wt% phosphoric acid solution is being continued under the stirring, spraying enters in the corn starch material bed granulates.
(6) granule sclerosis, the waterproof coating: after granulation was finished, dry 30min sprayed into the heat fused that atomizes, and temperature is 95 ℃ a stearic acid melt, and granule is carried out the waterproof coating, plays the granule induration simultaneously.
(7) granule enteric coating: after the stearic acid coating was finished, the preparation coating solution sprayed into atomizing polyacrylic resin alcoholic solution, and granule is carried out enteric coating.The alcoholic solution compound method of polyacrylic resin II and polyacrylic resin III such as embodiment 1.
(8) drying: dry materials 30min.
(9) cooling, packing: shut down, take out material, packing is cooled to 45 ℃ of temperature, crosses 10 mesh standard sieves, and metering packing gets finished product.
Three, Mercaptamine content detection:
Measure according to aforementioned cysteamine detection method of content, getting Mercaptamine content is 34.20wt%, and moisture is 5.44%.Follow the tracks of after 5 months, measuring Mercaptamine content is 34.15wt%, and moisture is 5.60%.
This product is faint yellow, has popcorn fragrance, graininess, and free-running property is good.
Embodiment 3
One, prescription:
54 kilograms of Mercaptamines;
52 kilograms of corn starchs
1.5 kilograms of vitamin Cs;
45 kilograms of glucoses;
10 kilograms of stearic acid;
5.5 kilograms of 85wt% phosphoric acid;
Above-mentioned raw materials all can be buied in raw materials market.
Two, the operating procedure step is as follows:
(1) Mercaptamine fusing: Mercaptamine, vitamin C splendid attire are in plastic containers, and boiling water bath is heated to fully and dissolves, and are heated to 83 ℃.
(2) add glucose powder, fusing: when the melt temperature reaches 83 ℃, add the food stage glucose powder, heat and be stirred to fully and dissolve, and be heated to 92 ℃.
(3) Mei Lade reaction: when the melt temperature reaches 92 ℃, in boiling water bath, heat while stirring, carry out Maillard reaction, response time 95min.
(4) cooling adds the 85wt% phosphoric acid solution: take out the plastics reaction vessel in the boiling water bath, put into lasting stirring of psychrolusia and be cooled to 55 ℃, add the 85wt% phosphoric acid solution while stirring, stir, guarantee that phosphoric acid is evenly distributed in the solution.
(5) granulate: drop into corn starch in cyclone fluidized bed, the Maillard reaction liquid that adds the 85wt% phosphoric acid solution is being continued under the stirring, spraying enters in the corn starch material bed granulates.
(6) granule sclerosis, the waterproof coating: after granulation was finished, dry 28min sprayed into the heat fused that atomizes, and temperature is 92 ℃ a stearic acid melt, and granule is carried out the waterproof coating, plays the granule induration simultaneously.
(7) granule enteric coating: after the stearic acid coating was finished, the preparation coating solution sprayed into atomizing polyacrylic resin alcoholic solution, and granule is carried out enteric coating.The alcoholic solution compound method of polyacrylic resin II and polyacrylic resin III such as embodiment 1.
(8) drying: dry materials 28min.
(9) cooling, packing: shut down, take out material, packing is cooled to 42 ℃ of temperature, crosses 10 mesh standard sieves, and metering packing gets finished product.
Three, Mercaptamine content detection:
Method according to aforementioned cysteamine content detection is measured, and getting Mercaptamine content is 33.02wt%, and moisture is 6.04%.Follow the tracks of after 5 months, measuring Mercaptamine content is 32.81wt%, and moisture is 6.74%.
This product is faint yellow, has popcorn fragrance, graininess, and free-running property is good.
Claims (5)
1. granulating coated slow release product of cysteamine hydrochloride by mass percentage, comprises following component:
Mercaptamine 31.5～35.6%
Corn starch 30.5～35.5%
Vitamin C 0.7～1.5%
Glucose powder 25.0～30%
Stearic acid 5.0～10.0%
85wt% phosphoric acid 2.0～4.0%.
2. granulating coated slow release product of cysteamine hydrochloride according to claim 1 is characterized in that, Mercaptamine content 〉=30.50wt% in the described product, moisture 0-8.0wt%.
3. the preparation method of granulating coated slow release product of cysteamine hydrochloride according to claim 1 and 2 may further comprise the steps:
(1) Mercaptamine fusing: Mercaptamine, vitamin C are pressed the described quality proportioning of claim 1 splendid attire in plastic containers, and the boiling water bath heating is stirred to fully and dissolves, and is heated to 80-85 ℃;
(2) add glucose powder and fusing: when the Mercaptamine melt reaches 80-85 ℃, add glucose powder, heated and stirred continues to be heated to 90-95 ℃ to dissolving fully;
(3) Maillard reaction: above-mentioned melt is heated while stirring in boiling water bath, carry out Maillard reaction 85-100min;
(4) cool off, add the 85wt% phosphoric acid solution: take out the Maillard reaction liquid container in the boiling water bath, put into psychrolusia, continue to stir, be cooled to 50-60 ℃, add the 85wt% phosphoric acid solution while stirring, stir;
(5) granulate: drop into corn starch in cyclone fluidized bed, add the above-mentioned Maillard reaction liquid that contains the 85wt% phosphoric acid solution, continuing under the stirring, spraying enters in the corn starch material bed granulates;
(6) granule sclerosis, waterproof coating: after granulation is finished, dry 20-30min, 90-100 ℃ of atomizing stearic acid melt carries out waterproof coating and granule sclerosis to granule;
(7) granule enteric coating: after the stearic acid coating was finished, the ethanol coating solution of atomizing polyacrylic resin carried out enteric coating to granule;
(8) cooling packing: after treating the dry 20-30min of above-mentioned granule materials, shut down, take out material, packing is cooled to 40-45 ℃, crosses 10 mesh standard sieves, and metering packing gets finished product.
4. preparation method according to claim 3 is characterized in that, described glucose and Mercaptamine are removed the stink and the bitterness of Mercaptamine itself through Maillard reaction under acid condition.
5. preparation method according to claim 3 is characterized in that, the agricultural liquid of described bag is the alcoholic solution of olefin(e) acid resin II in poly-and polyacrylic resin III.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102132768A (en) * | 2011-03-16 | 2011-07-27 | 江南大学 | Preparation method of cysteamine hydrochloride controlled-release feed additive |
| CN102240003A (en) * | 2010-05-14 | 2011-11-16 | 上海新农饲料有限公司 | Puffed full-fat soybean powder as well as preparation method and composition thereof |
| CN103005155A (en) * | 2013-02-05 | 2013-04-03 | 江南大学 | Preparation method for solid powder dog-food flavoring agent |
| CN103652366A (en) * | 2013-09-17 | 2014-03-26 | 杭州康德权饲料有限公司 | Stable mercaptamine enveloped by microcapsules and preparation method thereof |
| CN110664780A (en) * | 2013-06-17 | 2020-01-10 | 地平线孤儿病有限责任公司 | Delayed release cysteamine bead formulations, and methods of making and using the same |
-
2009
- 2009-11-09 CN CN2009101985705A patent/CN101703472B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240003A (en) * | 2010-05-14 | 2011-11-16 | 上海新农饲料有限公司 | Puffed full-fat soybean powder as well as preparation method and composition thereof |
| CN102132768A (en) * | 2011-03-16 | 2011-07-27 | 江南大学 | Preparation method of cysteamine hydrochloride controlled-release feed additive |
| CN102132768B (en) * | 2011-03-16 | 2012-08-29 | 江南大学 | Preparation method of cysteamine hydrochloride controlled-release feed additive |
| CN103005155A (en) * | 2013-02-05 | 2013-04-03 | 江南大学 | Preparation method for solid powder dog-food flavoring agent |
| CN110664780A (en) * | 2013-06-17 | 2020-01-10 | 地平线孤儿病有限责任公司 | Delayed release cysteamine bead formulations, and methods of making and using the same |
| CN110664780B (en) * | 2013-06-17 | 2022-09-27 | 地平线孤儿病有限责任公司 | Delayed release cysteamine bead formulations, and methods of making and using the same |
| CN103652366A (en) * | 2013-09-17 | 2014-03-26 | 杭州康德权饲料有限公司 | Stable mercaptamine enveloped by microcapsules and preparation method thereof |
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| CN101703472B (en) | 2011-06-22 |
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