CN104397361A - Preparation method for nanoscale colistin sulfate premix for feed - Google Patents

Preparation method for nanoscale colistin sulfate premix for feed Download PDF

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Publication number
CN104397361A
CN104397361A CN201410767202.9A CN201410767202A CN104397361A CN 104397361 A CN104397361 A CN 104397361A CN 201410767202 A CN201410767202 A CN 201410767202A CN 104397361 A CN104397361 A CN 104397361A
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colistine sulfate
preparation
feed
carry out
nanoscale
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CN201410767202.9A
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叶峰先
周玲
冯静波
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WUXI ZHENGDA POULTRY CO Ltd
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WUXI ZHENGDA POULTRY CO Ltd
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Abstract

A preparation method for a nanoscale colistin sulfate premix for a feed comprises the following steps: firstly, crushing the colistin sulfate raw material, adding water for dissolution, purifying, removing impurities, then enveloping the mixed solution, and finally, spray-drying to obtain the end product. The prepared nanoscale colistin sulfate premix is small in granularity, high in bioavailability and very remarkable in promoting growth.

Description

A kind of preparation method of feed nanoscale colistine sulfate pre-mixing agent
Technical field
The present invention relates to feed and field of feed additive technology, especially relate to a kind of production method of feed nanoscale colistine sulfate pre-mixing agent.
Background technology
Colistine sulfate has another name called Colistin (Colistin), aerosprin E (Polymyxin E), colistin etc., white or near-white powder, odorless, bitter, have draw moist, soluble in water, be slightly soluble in methyl alcohol, ethanol, be insoluble to acetone, ether etc., the aqueous solution is highly acid.
Colistine sulfate is produced by poly-viscosity bacillus, has stronger antibacterial action to Gram-negative bacteria, for the intestines problem that prevention and therapy Gram-negative bacteria causes, as feed addictive, and has obvious growth promoting function.But colistine sulfate is highly acid, and there is many alkaline matters in feed, as vitamin, trace element etc., easy and colistine sulfate reacts, and makes its decline of tiring, there is effect instability, and bioavailability declines.The hydrone reacting generation in addition can make feed water content improve, and feed easily goes bad, and period of storage shortens.
The medical material that current domestic veterinary drug enterprises uses especially antibiotic is all intermediate substantially, raw material producer is in order to reduce costs, only do the supernatant of fermentation aftertreatment technology, decolouring, dry, do not do purifying technique further, therefore finished product tire not high, such as colistine sulfate is tired basic about 1 milligram=22000 units, content only has about 73% (gravimetric method two kinds of unit conversions), fineness is at 60-80 order, 180-250 micron after converting, at the especially newborn baby pig feedstuff of animal feed, enter enteron aisle particle thick, diffusional area is little, bactericidal effect is limited.Purification not through the later stage is processed, and still containing a large amount of impurity, product quality does not reach the standard of imported raw material yet.Raiser, in breeding process, often needs in feed, add a large amount of colistine sulfate pre-mixing agents just effective.Antibiotic dosage is crossed conference and is brought medicament residue in animal body, has impact, after food chain transmission, finally also can produce negative consequence to health to animal late growing stage.
Summary of the invention
For the problems referred to above that prior art exists, the applicant provides a kind of preparation method of feed nanoscale colistine sulfate pre-mixing agent.Granularity of the present invention is little, bioavailability is high, growth promoting effects effect highly significant.
Technical scheme of the present invention is as follows:
A preparation method for feed nanoscale colistine sulfate pre-mixing agent, first pulverizes colistine sulfate raw material, is dissolved in water, purify, and remove impurity, then carry out bag quilt to mixed solution, last spraying dry obtains finished product.
Specifically comprise following processing step:
(1) colistine sulfate raw material input air flow micronizer is pulverized, obtain nanoscale colistine sulfate;
(2) pour the colistine sulfate crushed into reactor, be dissolved in water, carry out filtration and purify, remove impurity, then add oligoisomaltose and PVP and polyvinylpyrrolidone and carry out bag quilt;
(3) bag is carried out spraying dry by good colistine sulfate, obtain finished product.
Described pulverizing is dry type ultramicrotechnique, and smashing fineness is 5-10 micron, and crush efficiency is treating capacity 5-30kg/h.Describedly be dissolved in water, the weight ratio of water and colistine sulfate is 1-5:1.Described carry out wrapping by time, the weight ratio of colistine sulfate and capsulating material is 15:15-30.Described carry out wrapping by time, the temperature of coating buffer remains on 60-80 DEG C.Described spray-dired equipment is Highspeedcentrifugingandsprayingdrier, and drying process with atomizing condition is as follows: liquid supply speed: 10-20mlmin -1; EAT: 120-140 DEG C, leaving air temp: 25-60 DEG C, atomization gas flow velocity 300Lh -1.
The product finally obtained is the ultra-fine powder of almost spherical, and powder diameter is 5-10 μm.
The technique effect that the present invention is useful is:
The present invention's polymer substance wraps up colistine sulfate; colistine sulfate and external environment are isolated; both effectively tiring of colistin had been protected; improve stability; when colistin mixes with feed, also protect vitamin and alkalescence trace element in feed by the isolation of polymeric membrane and do not react with highly acid colistin, do not suffer a loss.
Fineness of the present invention reaches 5-10 μm, improves 25 times than common colistine sulfate fineness, and consumption reduces 3-5 doubly.After entering enteron aisle, polymeric membrane dissolves gradually, and colistin molecule also progressively discharges, and clinical trial result improves 3-5 doubly, can reduce times for spraying like this, reduces raiser's drug cost, increases economic efficiency.
And moisture of the present invention is less, appropriateness the feed shelf-life can be extended.Improve colistine sulfate bioavilability simultaneously, reduce times for spraying, reduce raiser's drug cost, increase economic efficiency.
Accompanying drawing explanation
Fig. 1 is production technological process of the present invention;
Fig. 2 ~ 5 are the picture of feed nanoscale colistine sulfate pre-mixing agent respectively under 50,100,150,200 times of height microscopes prepared by embodiment 1;
Fig. 6 is that the feed nanoscale colistine sulfate prepared of embodiment 1 and the relative surplus of common flour are tired (percentage) correlation curve.
Detailed description of the invention
Below in conjunction with the process chart shown in accompanying drawing 1, explain the present invention by specific embodiment.
Embodiment 1
Take the colistine sulfate raw material of 15kg, input air flow pulverizer, smashing fineness 5 μm is set, process about 30min, after terminating, colistine sulfate powder is dropped in the reactor of 2 tons, add the water-soluble solution of 2 times of weight, carry out filtration at the ultrafilter of liquid outlet to purify, remove impurity and heavy metal, the diameter of milipore filter is 450 μm, and the time is about 45min.Then add parcel capsule material oligoisomaltose 9kg, PVP9kg (temperature of coating buffer is 75 DEG C) and carry out bag quilt, after terminating, colistine sulfate and capsule material mixed solution are put spraying apparatus and carry out spraying dry, obtain colistine sulfate pre-mixing agent.Spraying apparatus is Highspeedcentrifugingandsprayingdrier, and drying process with atomizing condition is as follows: liquid supply speed: 10mlmin -1; EAT: 120 DEG C, leaving air temp: 25 DEG C, atomization gas flow velocity 300Lh -1, obtain the micro-capsule of almost spherical, micro-capsule diameter is 7 μm.
Embodiment 2
Take the colistine sulfate raw material of 15kg, input air flow pulverizer, smashing fineness 6 μm is set, process about 25min, after end, colistine sulfate powder is dropped in the reactor of 2 tons, add the water-soluble solution of 3 times of weight, carry out filtration at the ultrafilter of liquid outlet and purify, remove impurity and heavy metal, the diameter of milipore filter is 450 μm.Add parcel capsule material oligoisomaltose 12kg, PVP12kg (temperature of coating buffer is 76 DEG C) after processing about 30min and carry out bag quilt, after end, colistine sulfate and capsule material mixed solution are put spraying apparatus and carry out spraying dry, obtain colistine sulfate pre-mixing agent.Spraying apparatus is Highspeedcentrifugingandsprayingdrier, and drying process with atomizing condition is as follows: liquid supply speed: 15mlmin-1; EAT: 140 DEG C; Leaving air temp: 40 DEG C, atomization gas flow velocity 300Lh -1, obtain the micro-capsule of almost spherical, micro-capsule diameter is 8 μm.
Embodiment 3
Take the colistine sulfate raw material of 15kg, input air flow pulverizer, smashing fineness 7 μm is set, process about 20min, after end, colistine sulfate powder is dropped in the reactor of 2 tons, add the water-soluble solution of 4 times of weight, carry out filtration at the ultrafilter of liquid outlet and purify, remove impurity and heavy metal, the diameter of milipore filter is 450 μm.Add parcel capsule material oligoisomaltose 14kg, PVP14kg (temperature of coating buffer is 78 DEG C) after processing about 30min and carry out bag quilt, after end, colistine sulfate and capsule material mixed solution are put spraying apparatus and carry out spraying dry, obtain colistine sulfate pre-mixing agent.Spraying apparatus is Highspeedcentrifugingandsprayingdrier, and drying process with atomizing condition is as follows: liquid supply speed: 20mlmin -1; EAT: 140 DEG C, leaving air temp: 60 DEG C, atomization gas flow velocity 300Lh -1, obtain the micro-capsule of almost spherical, micro-capsule diameter is 9 μm.
Test example
1, the picture of the feed nanoscale colistine sulfate pre-mixing agent for preparing of embodiment 1 under 50,100,150,200 times of height microscopes as shown in Figure 2-5.
2, embodiment 1 is prepared feed nanoscale colistine sulfate and common flour (the colistine sulfate pre-mixing agent that sunlight Nutritional Technologies, INC. of Zhejiang Zhejiang University produces) and put into premix (the 4% young composite premixed feed for pig that Wuxi Zhengda Livestock Co., Ltd produces, formula is: corn 65kg, dregs of beans 26kg, wheat bran 5kg, colistine sulfate product 4kg) in, preserve 16 weeks under room temperature.The tire correlation curve of (percentage) of the colistine sulfate relative surplus of two kinds of raw materials (adopts antibiotic-microbial assay to detect) as shown in Figure 6.
As seen from Figure 6, the relative surplus of the feed nanoscale colistine sulfate that the present invention prepares is tired far above common flour, and this shows that this product has very high stability.
3, clinical testing:
Do experiment in the pig farm poor at many breeding environments,
Test period for the first time: on August 23rd, 2014 was to October 5.
Control group: the sucking pig 20 choosing 28 age in days diarrhoea, to feed piglet preweaning feed, child care material, add 10% common colistine sulfate (the colistin sulphate pre-mixing agent that sunlight Nutritional Technologies, INC. of Zhejiang Zhejiang University produces) 1.5kg in feed per ton, use 6 weeks continuously.
Test group: the sucking pig 20 choosing 28 age in days diarrhoea under equal rearing conditions, to feed identical piglet preweaning feed, child care material, add the nanoscale colistine sulfate 0.5kg (other compatibilities are constant) that 10% the present invention produces in feed per ton, use 6 weeks continuously.The diarrhea rate of control group, test group all has reduction, and control group have dropped 8.2%, and test group reduces 10.1%.
Second time test period: on October 25th, 2014 was to December 7.
Control group: the sucking pig 20 choosing 30 age in days diarrhoea, to feed piglet preweaning feed, child care material, add 10% common colistine sulfate (the colistin sulphate pre-mixing agent that sunlight Nutritional Technologies, INC. of Zhejiang Zhejiang University produces) 1.8kg in feed per ton, use 6 weeks continuously.
Test group: the sucking pig 20 choosing 30 age in days diarrhoea under equal rearing conditions, to feed identical piglet preweaning feed, child care material, add the nanoscale colistine sulfate 0.6kg (other compatibilities are constant) that 10% the present invention produces in feed per ton, use 6 weeks continuously.The diarrhea rate of control group, test group all has reduction, and control group have dropped 7.6%, and test group reduces 9.6%.
Colistine sulfate purified nanotubes bag is by technique, the bioavailability that can promote 5 times is proved through the demonstration of science and the productive experiment of reality, the dosage that can specify by Ministry of Agriculture's feed statutory standard adds, cost does not rise by original addition, solve feed factory exceed standard add problem and newborn intestine of young pigs diarrhoea problem.

Claims (7)

1. a feed preparation method for nanoscale colistine sulfate pre-mixing agent, is characterized in that first being pulverized by colistine sulfate raw material, is dissolved in water, purifies, and remove impurity, then carry out bag quilt to mixed solution, last spraying dry obtains finished product.
2. preparation method according to claim 1, is characterized in that specifically comprising following processing step:
(1) colistine sulfate raw material input air flow micronizer is pulverized, obtain nanoscale colistin sulphate;
(2) pour the colistine sulfate crushed into reactor, be dissolved in water, carry out filtration and purify, remove impurity, then add oligoisomaltose and PVP and polyvinylpyrrolidone and carry out bag quilt;
(3) bag is carried out spraying dry by good colistine sulfate, obtain finished product.
3. preparation method according to claim 1 and 2, it is characterized in that described pulverizing is dry type ultramicrotechnique, smashing fineness is 5-10 micron, and crush efficiency is treating capacity 5-30kg/h.
4. preparation method according to claim 1 and 2, in being dissolved in water described in it is characterized in that, the weight ratio of water and colistine sulfate is 1-5:1.
5. preparation method according to claim 1 and 2, carry out described in it is characterized in that wrapping by time, the weight ratio of colistine sulfate and capsulating material is 15:15-30.
6. preparation method according to claim 1 and 2, carry out described in it is characterized in that wrapping by time, the temperature of coating buffer remains on 60-80 DEG C.
7. preparation method according to claim 1 and 2, it is characterized in that described spray-dired equipment is Highspeedcentrifugingandsprayingdrier, drying process with atomizing condition is as follows: liquid supply speed: 10-20mlmin -1; EAT: 120-140 DEG C, leaving air temp: 25-60 DEG C, atomization gas flow velocity 300Lh -1.
CN201410767202.9A 2014-12-12 2014-12-12 Preparation method for nanoscale colistin sulfate premix for feed Pending CN104397361A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106376746A (en) * 2016-08-31 2017-02-08 无锡正大生物股份有限公司 Non-resistant piglet health premix and production method thereof
CN110801511A (en) * 2019-11-29 2020-02-18 广东容大生物股份有限公司 Colistin sulfate premix and preparation method thereof
CN111568864A (en) * 2020-06-01 2020-08-25 南京大方生物工程有限公司 Colistin sulfate soluble powder for improving solubility and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN1409638A (en) * 1999-12-14 2003-04-09 旭化成株式会社 Colistin sulfate granules
CN101664112A (en) * 2009-09-11 2010-03-10 无锡正大畜禽有限公司 Production method of feed colistin sulfate microcapsules
CN102258765A (en) * 2011-07-11 2011-11-30 浙江升华拜克生物股份有限公司 Preparation method of colistin sulfate premix
CN102600453A (en) * 2012-03-21 2012-07-25 江苏赛奥生化有限公司 Preparation method of colistin sulfate premixing agents
CN103641893A (en) * 2013-11-18 2014-03-19 宁夏泰瑞制药股份有限公司 Method for recovering colistin sulfate from colistin sulfate slag

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Publication number Priority date Publication date Assignee Title
CN1409638A (en) * 1999-12-14 2003-04-09 旭化成株式会社 Colistin sulfate granules
CN101664112A (en) * 2009-09-11 2010-03-10 无锡正大畜禽有限公司 Production method of feed colistin sulfate microcapsules
CN102258765A (en) * 2011-07-11 2011-11-30 浙江升华拜克生物股份有限公司 Preparation method of colistin sulfate premix
CN102600453A (en) * 2012-03-21 2012-07-25 江苏赛奥生化有限公司 Preparation method of colistin sulfate premixing agents
CN103641893A (en) * 2013-11-18 2014-03-19 宁夏泰瑞制药股份有限公司 Method for recovering colistin sulfate from colistin sulfate slag

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106376746A (en) * 2016-08-31 2017-02-08 无锡正大生物股份有限公司 Non-resistant piglet health premix and production method thereof
CN110801511A (en) * 2019-11-29 2020-02-18 广东容大生物股份有限公司 Colistin sulfate premix and preparation method thereof
WO2021103239A1 (en) * 2019-11-29 2021-06-03 广东容大生物股份有限公司 Colistin sulphate premix and preparation method therefor
CN110801511B (en) * 2019-11-29 2021-07-09 广东容大生物股份有限公司 Colistin sulfate premix and preparation method thereof
CN111568864A (en) * 2020-06-01 2020-08-25 南京大方生物工程有限公司 Colistin sulfate soluble powder for improving solubility and preparation method and application thereof
CN111568864B (en) * 2020-06-01 2022-06-24 南京大方生物工程有限公司 Colistin sulfate soluble powder capable of improving solubility and preparation method and application thereof

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Application publication date: 20150311