CN102579369B - Sodium butyrate enteric sustained release preparation and preparation method thereof - Google Patents

Sodium butyrate enteric sustained release preparation and preparation method thereof Download PDF

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CN102579369B
CN102579369B CN 201210092693 CN201210092693A CN102579369B CN 102579369 B CN102579369 B CN 102579369B CN 201210092693 CN201210092693 CN 201210092693 CN 201210092693 A CN201210092693 A CN 201210092693A CN 102579369 B CN102579369 B CN 102579369B
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sodium butyrate
sustained release
preparation
temperature
enteric sustained
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CN102579369A (en
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逯佩凤
周玉岩
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Hubei Hiyee Biological Technology Co ltd
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HUBEI NUOXIN BIO-TECHNOLOGY Co Ltd
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Abstract

The invention discloses a sodium butyrate enteric sustained release preparation and a preparation method thereof. The method comprises the following steps of: synthesizing sodium butyrate by a synthetic process, performing clathration on a synthesized sodium butyrate liquid in the liquid state, spraying and granulating to obtain the sodium butyrate enteric sustained release preparation. According to the method, production links and production cost are reduced, the influence of the production process on environment is reduced, and the volatile smell and hygroscopicity of the product are reduced; and the prepared sodium butyrate enteric sustained release preparation is white spherical particles, and the particle size is 200 to 500 micrometers. The sodium butyrate enteric sustained release preparation is high in stability and humidity resistance and can be released in intestinal tracts slowly, so that the bioavailability of the product is improved.

Description

Sodium butyrate enteric sustained release and preparation method thereof
Technical field
The invention belongs to field of medicaments, the present invention relates to a kind of sodium butyrate enteric sustained release and preparation method thereof.
Background technology
Sodium butyrate is the organic acid sodium salt of short-chain fatty acid, has the breeding performonce fo animals of improvement, regulating intestinal canal flora structure of community, keeps the multiple effects such as intestinal normal morphology and enhancing human body immunity function.
Sodium butyrate is extensively made an addition in the animal and fowl fodder to improve the health level of poultry as a kind of green, non-harmful feed additive, improves food conversion ratio and economic benefit.But the sample gas flavor because the strong cheese of sodium butyrate tool becomes sour, the site operation personnel is difficult to adapt to when the production of sodium butyrate and use, and larger on producing with the air ambient impact in use zone; Drawing that the sodium butyrate tool is stronger is moist, and easily moisture absorption knot is fast, is not easy to preserve.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of method for preparing sodium butyrate enteric sustained release, and the method reduces the production link of sodium butyrate, reduces its volatile flavor, and the sodium butyrate enteric sustained release of preparation draws moist reduction.
The technical scheme that solves the problems of the technologies described above is:
A kind of method for preparing sodium butyrate enteric sustained release may further comprise the steps:
(1) with dissolution of sodium hydroxide in water, at the uniform velocity drip n-butyric acie, dropwise and continue reaction 0.8-1.2 hour, get the sodium butyrate reactant liquor; The mass ratio of sodium hydroxide and n-butyric acie is 7: 15-17;
(2) add adjuvant in above-mentioned sodium butyrate reactant liquor, described adjuvant is one or both and one or more the mixture that is selected from ethyl cellulose, hydroxypropyl cellulose, methacrylic acid, acrylate copolymer, propylene glycol, polypropylene glycol, mono stearate glyceryl ester, the beta cyclodextrin in polyacrylic resin, the acrylic resin; The amount of described adjuvant is that the mass ratio with sodium butyrate is 125-500: 500;
(3) with the material in (2), emulsification pretreatment 10-20 minute, temperature was controlled to be 45~65 ℃;
(4) material behind the emulsification pretreatment in the step (3) is imported in the centrifugal atomizer, 5000~6000 rev/mins of atomizing disk rotating speeds, temperature is 180~200 ℃ of spray granulation;
(5) cooling, concussion is sieved, and collects, and namely gets sodium butyrate enteric sustained release.
Among embodiment, in the step (1), the temperature when dripping n-butyric acie is 48 ℃-55 ℃ therein; The time that drips n-butyric acie is 1.8-2.3 hour; The temperature of reaction is 50 ℃-75 ℃, and pH is between 7.0 to 7.5 in control.
Among embodiment, the mass ratio of sodium hydroxide and n-butyric acie is 7: 16 therein, and the temperature of reaction is 50 ℃-55 ℃.
Therein among embodiment, the amount of described adjuvant is that the mass ratio with sodium butyrate is 125: 500.
Among embodiment, described adjuvant is the mixture of polyacrylic resin, propylene glycol, glyceryl monostearate and ethyl cellulose therein.
Among embodiment, the emulsification pretreatment temperature is 45 ℃-55 ℃ in the step (3) therein.
Another technical issues that need to address of the present invention provide a kind of sodium butyrate enteric sustained release.
The technical scheme that solves the problems of the technologies described above is:
According to the sodium butyrate enteric sustained release that said method is prepared into, wherein, the quality percentage composition of adjuvant is 20%-50%, and the quality percentage composition of sodium butyrate contains and is 50%-80%.
Among embodiment, sodium butyrate enteric sustained release is white spheroidal particle therein, and size is 200 μ m-500 μ m.
The present invention is directed to and change existing sodium butyrate production synthetic butyric acid sodium raw materials (powder), again sodium butyrate is produced ordinary preparation or peplos preparation, reduce sodium butyrate production link, production cost and production process to the impact of environment, from the sodium butyrate synthesis technique, synthetic sodium butyrate liquid is carried out enclose under the liquid state, behind the liquid enclose with suitable preparation parameter, spray granulation reduces the volatile flavor of product and draws moist.
The preparation method of sodium butyrate enclose preparation of the present invention is simple, cost is low, easy to operate, loss is few, and total yield of products is high, reduced the distinctive abnormal flavour of sodium butyrate in the production environment, the sodium butyrate enclose preparation outward appearance that its production the obtains spheroidal particle that is white in color, microscopically is viewed as translucent, size 200 μ m-500 μ m, good fluidity, the intestinal dissolving.By preparation method provided by the invention, in conjunction with selected adjuvant, the sodium butyrate preparation that obtains is compared with plain particles has significant improvement, mainly contains: synthetic, one step of preparation finishes; Used adjuvant is simple, has effectively reduced the abnormal flavour that product produces in production and application process; Good stability, humidity resistance is strong, can slowly discharge in gastrointestinal, improved the bioavailability of product.
Description of drawings
Fig. 1 is sodium butyrate agent enclose of the present invention flow chart processed;
Fig. 2 is schematic diagram under the sodium butyrate microscope of the present invention (40 times);
Description of reference numerals
1, No. 1 retort, 2, No. 2 retort, 3, the purified water measuring tank, 4, elevated dosing vessel, 5, the spray tower, 6 double-deck shaking screens.
The specific embodiment
Below by specific embodiment, by reference to the accompanying drawings, the present invention will be further described.
Embodiment one
(1) referring to Fig. 1, suction 400kg purified water joins in No. 1 retort 1 from purified water measuring tank 3, opens and stirs, slowly drop into the 175kg sodium hydroxide, fully after the dissolving, in No. 2 retort 2 of suction, ON cycle water management temperature is (48-50 ℃) about 50 ℃;
(2) add the 400kg n-butyric acie to 500L elevated dosing vessel 4, at the uniform velocity drop to again in No. 2 retort 2, use circulating water cooling control temperature the highest not above 85 ℃, dripped with 2 hours, solution temperature when dripping n-butyric acie is 48-50 ℃, dropwises to continue reaction 1 hour, and the temperature of reaction is 50~55 ℃, pH is between 7.0 to 7.5 in control, obtains the sodium butyrate reaction solution;
(3) add ethyl cellulose 25kg, polyacrylic resin (being purchased from the mountains and rivers, Anhui pharmaceutic adjuvant limited company) 93kg, propylene glycol 2kg, glyceryl monostearate (being purchased from Guangzhou Kevin Food Co., Ltd.) 5kg at above-mentioned sodium butyrate reaction solution (approximately containing sodium butyrate 500kg), emulsification pretreatment 10-20 minute, temperature was controlled to be 45~55 ℃;
(4) material after the emulsifying is imported in the centrifugal atomizer of spray tower 5,5000~5500 rev/mins of atomizing disk rotating speeds, temperature is 180~200 ℃ of spray granulation;
(5) cooling, with made finished particle with the collection of sieving of 4~No. 6 (aperture 30~80 orders) double-deck shaking screens 6.Obtain at last 625kg sodium butyrate enteric sustained release (content of adjuvant is 20%, the content of sodium butyrate approximately 80%), particle diameter is at 200 μ m-500 μ m, and yield can reach 98%.As shown in Figure 2, the sodium butyrate preparation is translucent under 40 power microscopes, white spheroidal particle.
Embodiment two
(1) suction 400kg purified water joins in No. 1 retort 1 from purified water measuring tank 3, opens and stirs, and slowly drops into the 175kg sodium hydroxide, and fully after the dissolving, in No. 2 retort 2 of suction, ON cycle water management temperature is about 50 ℃;
(2) add the 400kg n-butyric acie to 500L elevated dosing vessel 4, at the uniform velocity drop in No. 2 retort 2, use that circulating water cooling control temperature is the highest to surpass 85 ℃, drip with 1.8 hours, the solution temperature during the dropping n-butyric acie is controlled to be 50-55 ℃; Dropwise and continue reaction 1 hour, pH is between 7.0 to 7.5 in control, and the temperature of reaction is 65-70 ℃, obtains the sodium butyrate reaction solution;
(3) above-mentioned reactant liquor (approximately containing sodium butyrate 500kg) is added ethyl cellulose 5kg, polyacrylic resin 50kg, polypropylene glycol 3kg, glyceryl monostearate 10kg, beta cyclodextrin 432kg, emulsification pretreatment 10-20 minute, temperature was controlled to be 55 ℃-65 ℃;
(4) material after the emulsifying is imported in the centrifugal atomizer of spray tower, 5500~6000 rev/mins of atomizing disk rotating speeds, temperature is 180~200 ℃ of spray granulation;
(5) cooling, with made finished particle with the collection of sieving of 4~No. 6 double-deck shaking screens.Obtain at last 1000kg sodium butyrate preparation (content of adjuvant is about 50%, the content 50% of sodium butyrate), particle diameter is at 200 μ m-500 μ m, and yield can reach 99%.Microscope (40 times) testing result is identical with embodiment 1, and as shown in Figure 2, the sodium butyrate preparation is translucent under 40 power microscopes, white spheroidal particle.
Embodiment three
(1) suction 400kg purified water joins in No. 1 retort 1 from purified water measuring tank 3, opens and stirs, and slowly drops into the 175kg sodium hydroxide, and fully after the dissolving, in No. 2 retort of suction, ON cycle water management temperature is about 50 ℃;
(2) add the 400kg n-butyric acie to the 500L elevated dosing vessel, at the uniform velocity drop in the retort, use that circulating water cooling control temperature is the highest to surpass 85 ℃, drip with 2 hours, the temperature of the solution during the dropping n-butyric acie is 48-55 ℃; Dropwise and continue reaction 1.2 hours, the temperature of reaction is 50~55 ℃, and pH is between 7.0 to 7.5 in control, obtains the sodium butyrate reaction solution;
(3) above-mentioned reactant liquor (approximately containing sodium butyrate 500kg) is added ethyl cellulose 5kg, polyacrylic resin 50kg, propylene glycol 5kg, glyceryl monostearate 20kg, beta cyclodextrin 253kg, emulsification pretreatment 10-20 minute, temperature was controlled to be 45 ℃~55 ℃;
(4) material after the emulsifying is imported in the centrifugal atomizer of spray tower, 5000~5500 rev/mins of atomizing disk rotating speeds, temperature is 180~200 ℃ of spray granulation
(5) cooling, with made finished particle with the collection of sieving of 4~No. 6 double-deck shaking screens.Obtain at last 832kg sodium butyrate preparation (content of adjuvant is 40%, and the content of sodium butyrate is 60%), particle diameter is at 200 μ m-500 μ m, and yield can reach 99%.Microscope (40 times) testing result is identical with embodiment 1, and as shown in Figure 2, the sodium butyrate preparation is translucent under 40 power microscopes, white spheroidal particle.
Embodiment four
1, draws moist comparison: take by weighing weighing sample 10 grams, put in the uncovered weighing botle, place (temperature 22~25 degree, humidity 65~80% under the room temperature state, respectively 0,30,60 ... sampling in 600 minutes claims its weight, determines whether to draw wet and how much hygroscopic.The sodium butyrate preparation and the city's pin sodium butyrate plain particles that prepare in embodiment one, example two, the example three are drawn moist comparison, and comparative result sees attached list.
Figure BDA0000149611270000061
2, drug release determination: with reference to 117 pages of two appendix of " Chinese veterinary pharmacopoeia " version in 2010, the second method, method 1 in the drug release determination method) mensuration product release, getting product an amount of (being equivalent to sodium butyrate 3g) among the embodiment places and turns basket, according to take 0.1mol/L hydrochloric acid solution 750ml as dissolution medium, rotating speed is that per minute 100 turns, temperature is 37 ℃, in accordance with the law operation, got solution 25ml in 2 hours, replenish simultaneously the dissolution medium of equal volume, use less than 0.45 μ m filter membrane to filter, precision measures the 20ml oven drying at low temperature to constant weight, and is for subsequent use; 2 hours finish, add immediately 0.2mol/L sodium radio-phosphate,P-32 solution 250ml (regulating pH value to 6.8 ± 0.05 with 2mol/L hydrochloric acid solution or 2mol/L sodium radio-phosphate,P-32 solution in case of necessity), remain in operation, 2, got solution 25ml in 4,6 hours, replenish simultaneously dissolution medium (750 hydrochloric acid solutions: 250 sodium radio-phosphate,P-32 solutions) of equal volume, use less than 0.45 μ m filter membrane to filter, get oven drying at low temperature to constant weight, for subsequent use; The above-mentioned sample for preparing is added respectively water 25ml heated and boiled dissolving, and methylate is red-3 of bromocresol green index liquid, is titrated to solution with hydrochloric acid volumetric solution (0.1mol/L) and shows redness and be terminal point, and the result proofreaies and correct with blank assay.Calculate content, must not cross 30% of labelled amount in 2 hours in 0.1mol/L hydrochloric acid solution release, at 2 hours labelled amounts about 70% of pH6.8 buffer release, 4 hours labelled amounts about 80%, 6 hours labelled amount 95% left and right sides %.
Every 1ml hydrochloric acid volumetric solution (0.1mol/L) is equivalent to the sodium butyrate of 11.01mg.
Computing formula: labelled amount (%)=V*F*0.01101* extension rate/sampling amount/labelled amount testing result:
The drug release determination result of sodium butyrate
Figure BDA0000149611270000071
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (1)

1. method for preparing sodium butyrate enteric sustained release is characterized in that: may further comprise the steps:
(1) with dissolution of sodium hydroxide in water, at the uniform velocity drip n-butyric acie, dropwise and continue reaction 0.8-1.2 hour, get the sodium butyrate reactant liquor; The mass ratio of sodium hydroxide and n-butyric acie is 7:15-17;
(2) add adjuvant in above-mentioned sodium butyrate reactant liquor, described adjuvant is one or both and one or more the mixture that is selected from ethyl cellulose, hydroxypropyl cellulose, methacrylic acid, acrylate copolymer, propylene glycol, polypropylene glycol, mono stearate glyceryl ester, the beta cyclodextrin in polyacrylic resin, the acrylic resin; The amount of described adjuvant is that the mass ratio with sodium butyrate is 125-500:500;
(3) with the material in (2), emulsification pretreatment 10-20 minute, temperature was controlled to be 45~65 ℃;
(4) material behind the emulsification pretreatment in the step (3) is imported in the centrifugal atomizer of spray tower, 5000 ~ 6000 rev/mins of atomizing disk rotating speeds, temperature is 180~200 ℃ of spray granulation;
Cooling, concussion is sieved, and collects, and namely gets sodium butyrate enteric sustained release.
2, preparation method according to claim 1 is characterized in that, in the step (1), is just dripping
The temperature of solution is 48 ℃-55 ℃ during butanoic acid; The time that drips n-butyric acie is 1.8-2.3 hour; The temperature of reaction is 50 ℃-70 ℃, and pH is controlled between 7.0 to 7.5.
3, preparation method according to claim 1 is characterized in that, the mass ratio of described sodium hydroxide and n-butyric acie is 7:16, and the temperature of reaction is 50 ℃-55 ℃.
4, according to claim 1 each described preparation method is characterized in that-3, and described adjuvant is the mixture of polyacrylic resin, propylene glycol, glyceryl monostearate and ethyl cellulose.
5, according to claim 1 each described preparation method is characterized in that-3, and the emulsification pretreatment temperature is 45 ℃-55 ℃ in the step (3).
6, according to claim 1 each described preparation method is characterized in that-3, and the amount of described adjuvant is that the mass ratio with sodium butyrate is 125:500.
7, according to claim 1 the sodium butyrate enteric sustained release that is prepared into of each described method-5, the quality percentage composition of adjuvant is 20%-50%, the quality percentage composition of sodium butyrate is 50%-80%.
8, described sodium butyrate enteric sustained release according to claim 7 is characterized in that described sodium butyrate enteric sustained release is white spheroidal particle, size 200 μ m-500 μ m.
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CN105995192B (en) * 2016-05-17 2019-05-10 长沙学院 A kind of preparation method and application of feed of grass carp nano controlled-release sodium butyrate
CN106509368B (en) * 2016-09-19 2019-08-09 湖北神舟化工有限公司 A kind of preparation method of feed pellet type sodium butyrate
CN114468137A (en) * 2022-01-19 2022-05-13 浙江惠嘉生物科技股份有限公司 Sodium butyrate synthesis and microcapsule secondary coating preparation method
CN115245493A (en) * 2022-05-06 2022-10-28 福建医科大学附属协和医院 Sodium butyrate sustained-release tablet for delaying vascular aging

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