CN104161192B - A kind of preparation method of Thymol feed addictive - Google Patents
A kind of preparation method of Thymol feed addictive Download PDFInfo
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- CN104161192B CN104161192B CN201410282636.XA CN201410282636A CN104161192B CN 104161192 B CN104161192 B CN 104161192B CN 201410282636 A CN201410282636 A CN 201410282636A CN 104161192 B CN104161192 B CN 104161192B
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- thymol
- polyvinylpyrrolidone
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- mixed liquor
- feed addictive
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Abstract
The invention discloses a kind of preparation method of efficient Thymol feed addictive, the present invention has made the solid dispersions of polyvinylpyrrolidone and Thymol by solid dispersing technology, because macromolecular polyvinylpyrrolidone can be associated with micromolecular Thymol formation molecule, thereby reduce the volatility of Thymol raw material, simultaneously because polyvinylpyrrolidone has well water-soluble, in the time that solid dispersions is met water, polyvinylpyrrolidone dissolves fast, thereby discharge the Thymol of molecular state, solubility and the bioavilability of Thymol are significantly improved, therefore improved the action effect of Thymol.
Description
Technical field
The present invention relates to a kind of preparation method of feed addictive, particularly a kind of preparation method of efficient Thymol feed addictive.
Background technology
Thymol claims again thymol, because it is to separate and gained the name in grass from hundred at first. Thymol chemical name is thymol, chemical formula C10H14O, molecular weight 150.22, is that white is to light yellow crystalline powder under normal temperature. Thymol has thyme or hundred li of careless peat-reeks, is a kind of important source material of preparing menthol, is also usually used in the formula of toothpaste, some cosmetics of perfumed soap level. The effects such as that Thymol has is antibacterial, anticorrosion, anti-oxidant, antithrombotic, are used for oral hygiene, process wound, pest repellant etc. The application study of Thymol in feed is in recent years also more and more, Dorman and Dean(2000) research also shows that Thymol has stronger antibacterial action. Liao Fang etc. (2005) study and show, Thymol all has stronger restraining and sterilizing bacteria effect to enteritis common bacteria and shigella dysenteriae. Trevisi etc. (2010) have studied the impact of Thymol on piglet growth performance before and after salmonella infection and body temperature situation, and result shows that in feed, adding Thymol can improve word material conversion ratio. Luna etc. (2010) give broiler feeding Thymol, and result shows that Thymol can improve the meat of broiler chicken, reduce oxidation reaction. Cao Jianguo etc. (2004) find that Thymol can suppress other bad smell in word material, strengthen the palatability of diet, slow down the growth of bacterium in feed, maintain the quantity of profitable strain in enteron aisle, suppress pathogen, reduce the generation of enteron aisle diarrhoea, promote the Fast Growth of piglet. The researchs such as Li (2012) show that Feeding grain adds the coated plants essential oil (main component is Thymol and cinnamic acid) of 100mg/kg maltodextrin and significantly reduces grice diarrhoea index. Adopt the coated method of maltodextrin, its shortcoming is that in process of producing product, effective ingredient heat loss is large, energy consumption is very large, needs large-scale spray drying device, and equipment investment is large.
The green feed additive of the substitute antibiotics using as the approval of the current Ministry of Agriculture, Thymol is because of its green, environmental protection, antibacterial feature, makes its application in feed have good prospect. But Thymol is fat melting material, the dissolubility in water is poor, and in animal and bird intestines, effectively stripping of phoenix, has therefore affected its action effect, therefore improves the water-soluble significant to its action effect of Thymol. The method of hundred fragrant phenol preparations of current production is generally produced with simple premixing process, or is adsorbed on silica supports with liquid condition spraying after being heated. These processing technologys exist significantly not enough:
(1) Thymol belongs to plants essential oil, volatile in production, storage and use procedure, causes a large amount of losses of effective ingredient.
(2) Thymol belongs to plants essential oil, make an addition in feed after feed intake, to be difficult for absorbing or can not be miscible with the complete homogeneous of chyme in enteron aisle, thereby its fungistatic effect obviously reduces.
(3), because plants essential oil and water can not be miscible, therefore Thymol preparation cannot be used for drinking water for animals and adds, and has restricted the scope of application of product.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of efficient Thymol feed addictive, the preparation technology who utilizes solid dispersions by being insoluble in water, volatile Thymol raw material preparation becomes Thymol preparation soluble in water, reduce its volatility simultaneously, thereby improve the action effect of Thymol.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for efficient Thymol feed addictive, comprises the following steps:
(1) raw material Thymol and water soluble adjuvant polyvinylpyrrolidone are added in ethanolic solution, be uniformly mixed to obtain mixed liquor;
(2) mixed liquor leaves standstill after 10-20min, filters and removes insoluble impurities;
(3) step (2) mixed liquor after treatment vacuum drying 8-12h at 40-50 DEG C is obtained to chip solid thing, reclaim ethanol simultaneously;
(4) by the whole grain of oscillating granulator for chip solid thing, obtain particle diameter 40-80 object product.
As preferably, in step (1), the mass concentration of ethanolic solution is greater than 95%. The mass concentration of controlling ethanolic solution is greater than 95%, and Thymol dissolubility is good like this, is uniformly dispersed.
As preferably, in step (1), the quality proportioning of Thymol and polyvinylpyrrolidone is: Thymol 10-40%, polyvinylpyrrolidone 60%-90%, summation 100%. The ratio of controlling Thymol and polyvinylpyrrolidone, guarantees to make good water soluble preparation, if the ratio of polyvinylpyrrolidone and Thymol is 1:1, is unfavorable for making water soluble preparation, because the amount of water soluble adjuvant very little.
As preferably, the gross weight of Thymol and polyvinylpyrrolidone in step (1): the weight=1:2-4 of ethanolic solution. Control the gross weight of Thymol and polyvinylpyrrolidone: the weight=1:2-4 of ethanolic solution, so that polyvinylpyrrolidone and Thymol can whole molten ethanolic solutions.
As preferably, in step (1), speed of agitator is 30-60 rev/min.
As preferably, in step (2), filtering screen cloth used is 60-200 eye mesh screen.
As preferably, in step (3), vacuum is-0.07 ~-0.09Mpa.
The invention has the beneficial effects as follows:
1. the present invention has made the solid dispersions of polyvinylpyrrolidone and Thymol by solid dispersing technology, due to interweaving mutually of macromolecular polyvinylpyrrolidone and micromolecular Thymol, form molecule crosslinked state, thereby stop the volatilization of Thymol raw material, simultaneously because polyvinylpyrrolidone has well water-soluble, in the time that solid dispersions is met water, polyvinylpyrrolidone dissolves fast, thereby discharge the Thymol of molecular forms, significantly improve the solubility of Thymol, make the Thymol can be miscible with chyme homogeneous in enteron aisle, improve its bioavilability, therefore can increase the action effect of Thymol.
2. technique of the present invention is simple, easy operating. Equipment used in the present invention is conventional equipment, and handling safety is simple.
3. output of the present invention is higher, is easy to amplify, and equipment price is lower. Be suitable for high strength, large-scale production.
4. power is little in process of production in the present invention, because alcohol almost all reclaims, pollutes little.
5. product yield is high, and product yield is greater than 99%.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, raw material and the equipment etc. adopting all can be buied from market or this area is conventional. Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1:
A preparation method for efficient Thymol feed addictive, comprises the following steps:
(1) raw material Thymol 10 weight portions and water soluble adjuvant polyvinylpyrrolidone 90 weight portions are added in 200 weight portion absolute ethyl alcohols, it is mixed liquor that 30 revs/min of rotating speeds be uniformly mixed 20 minutes to make its solution that is dissolved as clarification.
(2) mixed liquor leaves standstill 10min, makes the contamination precipitation in former, auxiliary material, crosses 60 eye mesh screens and removes insoluble impurities.
(3) step (2) mixed liquor after treatment is placed in vacuum drying chamber, vacuum drying chamber is equipped with alcohol recovery device, and under 40 DEG C, the condition of vacuum-0.07Mpa, vacuum drying 12h obtains chip solid thing, reclaims ethanol simultaneously.
(4) by chip solid whole grain of oscillating granulator (model YK160) for thing, obtain particle diameter 40-80 object product.
Embodiment 2:
A preparation method for efficient Thymol feed addictive, comprises the following steps:
(1) raw material Thymol 40 weight portions and water soluble adjuvant polyvinylpyrrolidone 60 weight portions are added in 400 weight portion absolute ethyl alcohols, it is mixed liquor that 60 revs/min of rotating speeds be uniformly mixed 10 minutes to make its solution that is dissolved as clarification.
(2) mixed liquor leaves standstill 20min, makes the contamination precipitation in former, auxiliary material, crosses 200 eye mesh screens and removes insoluble impurities.
(3) step (2) mixed liquor after treatment is placed in vacuum drying chamber, vacuum drying chamber is equipped with alcohol recovery device, and under 50 DEG C, the condition of vacuum-0.09Mpa, vacuum drying 8h obtains chip solid thing, reclaims ethanol simultaneously.
(4) by chip solid whole grain of oscillating granulator (model YK160) for thing, obtain particle diameter 40-80 object product.
Embodiment 3:
A preparation method for efficient Thymol feed addictive, comprises the following steps:
(1) raw material Thymol 20 weight portions and water soluble adjuvant polyvinylpyrrolidone 80 weight portions are added in 300 weight portion absolute ethyl alcohols, it is mixed liquor that 50 revs/min of rotating speeds be uniformly mixed 15 minutes to make its solution that is dissolved as clarification.
(2) mixed liquor leaves standstill 15min, makes the contamination precipitation in former, auxiliary material, crosses 100 eye mesh screens and removes insoluble impurities.
(3) step (2) mixed liquor after treatment is placed in vacuum drying chamber, vacuum drying chamber is equipped with alcohol recovery device, and under 45 DEG C, the condition of vacuum-0.08Mpa, vacuum drying 10h obtains chip solid thing, reclaims ethanol simultaneously.
(4) by chip solid whole grain of oscillating granulator (model YK160) for thing, obtain particle diameter 40-80 object product.
Dissolution determination
Adopt the external method that manually simulates gastrointestinal tract environment to measure the dissolution rate of different Thymol additives, common Thymol treated end and the efficient Thymol preparation made by the present invention are added respectively to artificial simulation gastric juices by same content, 37 DEG C of reaction 2h, sampling, measure Thymol content in artificial simulation gastric juices, and then adjusting pH value to 6.8, form artificial simulation intestinal juice, 37 DEG C are continued reaction 2h, sampling, measure Thymol content in simulated intestinal fluid, measurement result is in table 1:
The dissolution rate of the efficient Thymol that the former powder of table 1 Thymol and the present invention make
Effect
Efficient Thymol feed addictive of the present invention had carried out animal experiment, and result shows to add in weanling pig daily ration average daily gain that the efficient Thymol feed addictive of the present invention can significantly improve weanling pig, reduces Escherichia coli quantity in ight soil.
120 of DLY piglets choosing 21 ± 2 ages in days wean, the principle identical in parity, body weight is close, male and female ratio is basically identical is divided into 3 groups: control group, common Thymol group, efficient Thymol group, every group of 4 repetitions, 10 pigs of each repetition. Control group Diet basal diet, does not add Thymol; Common Thymol group is added the common Thymol product (commercial) of 50mg/kg end through preparation processing in basal diet; Efficient Thymol group is added 50mg/kg efficient Thymol of the present invention in basal diet. Each group test pig environmental condition is consistent, and free choice feeding, freely drinks water, and other feeding and management is undertaken by pig farm routine. Feeding experiment 28 days by a definite date, records feed intake every day, and when 28 ages and 49 age in days, measure on an empty stomach the body weight of every piglet early morning, calculates average daily gain, average daily ingestion amount and material anharmonic ratio. When 49 age in days, every group is selected 6 healthy test pig, adopts rectum to get excrement method and collects excrement sample, measures excrement sample Bacillus acidi lactici, Bifidobacterium and Escherichia coli quantity, and result of the test is as table 2 and table 3:
Table 2: the impact of different Thymol products on Growth Performance of Weaning Piglets
Note: with a line acceptance of the bid different letter representation significant differences of note (P < 0.05), data coding method is average ± standard deviation.
Result of the test shows: the efficient Thymol preparation that in feed, interpolation is produced by embodiment of the present invention can significantly improve the average daily gain of weanling pig, efficient Thymol preparation group average daily gain improves 6.08%(P < 0.05 than control group and common Thymol group respectively) and 4.37%(P < 0.05), add the average daily gain of common Thymol group and be slightly improved than control group, but difference is not remarkable. Presentation of results can significantly improve the action effect of Thymol by the present invention.
Impact (the unit: log of the different Thymol products of table 2 on weanling pig faecal bacterial community10cfu/g）
| Group | Control group | Common Thymol group | Efficient Thymol group |
| Escherichia coli | 8.35±0.27a | 8.06±0.38a | 7.26±0.29b |
| Bacillus acidi lactici | 8.66±0.35 | 8.79±0.49 | 8.93±0.36 |
| Bifidobacterium | 9.11±0.39 | 9.25±0.39 | 9.38±0.39 |
Note: with a line acceptance of the bid different letter representation significant differences of note (P < 0.05), data coding method is average ± standard deviation.
Result of the test shows: in feed, add the efficient Thymol preparation of producing by embodiment of the present invention and can significantly reduce colibacillary quantity in excrement sample, and beneficial bacterium Bacillus acidi lactici and Bifidobacterium are not made significant difference.
Above-described embodiment is preferably scheme of one of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.
Claims (4)
1. a preparation method for Thymol feed addictive, is characterized in that, comprises the following steps:
(1) raw material Thymol and water soluble adjuvant polyvinylpyrrolidone are added in ethanolic solution, be uniformly mixed to obtain mixed liquor;
(2) mixed liquor leaves standstill after 10-20min, filters and removes insoluble impurities;
(3) step (2) mixed liquor after treatment vacuum drying 8-12h at 40-50 DEG C is obtained to chip solid thing, reclaim ethanol simultaneously;
(4) by the whole grain of oscillating granulator for chip solid thing, obtain particle diameter 40-80 object product;
In step (1), the mass concentration of ethanolic solution is greater than 95%; In step (1), the quality proportioning of Thymol and polyvinylpyrrolidone is: Thymol 10-40%, polyvinylpyrrolidone 60%-90%, summation 100%; The gross weight of Thymol and polyvinylpyrrolidone in step (1): the weight=1:2-4 of ethanolic solution.
2. preparation method according to claim 1, is characterized in that: in step (1), speed of agitator is 30-60 rev/min.
3. preparation method according to claim 1, is characterized in that: in step (2), filtering screen cloth used is 60-200 eye mesh screen.
4. preparation method according to claim 1, is characterized in that: in step (3), vacuum is-0.07 ~-0.09Mpa.
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| CN105815572A (en) * | 2016-03-21 | 2016-08-03 | 浙江日出生物科技有限公司 | Antimicrobial compound acidifier |
| CN107496361B (en) * | 2017-08-11 | 2020-08-18 | 浙江工业大学 | Thyme essential oil solid dispersion and preparation method thereof |
| CN111329873A (en) * | 2018-12-19 | 2020-06-26 | 成都华罗生物科技有限公司 | Pharmaceutical composition for improving growth performance of pigs as well as preparation method and application thereof |
| CN112998133B (en) * | 2021-02-24 | 2022-08-23 | 中国科学院上海药物研究所 | Plant essential oil amino acid composition and preparation method thereof |
| CN113712119A (en) * | 2021-08-20 | 2021-11-30 | 江苏康雅生物科技有限公司 | Cinnamic aldehyde coating premixed preparation for livestock and poultry and preparation method thereof |
| CN115428869B (en) * | 2022-09-02 | 2024-01-05 | 南京农业大学 | Biological agent for improving intestinal health of broiler chickens and preparation method and application thereof |
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| SE9801742L (en) * | 1998-05-18 | 1999-11-19 | Akzo Nobel Nv | Use of natural substances containing thymol in the preparation of animal feed |
| CN101502553B (en) * | 2008-12-19 | 2013-04-10 | 深圳海创医药科技发展有限公司 | Rhizoma atractylodis total terpene alcohol solid dispersoid, medicament composition and preparation method thereof |
| CN102132764B (en) * | 2011-03-02 | 2013-09-04 | 广州英赛特生物技术有限公司 | Application of para-thymol, salts ramification thereof or esters ramification thereof in animal feed additive |
| CN102178061A (en) * | 2011-05-11 | 2011-09-14 | 张奎昌 | Method for preparing origanum oil-beta-cyclodextrin inclusion compound feed additive |
| CN102935110B (en) * | 2012-11-02 | 2014-08-06 | 青岛蔚蓝生物股份有限公司 | Coated granules containing natural oregano oil for birds and preparation method thereof |
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Denomination of invention: A kind of preparation method of thymol feed additive Effective date of registration: 20220906 Granted publication date: 20160504 Pledgee: Zhejiang Anji Rural Commercial Bank of the West Branch of Limited by Share Ltd. Pledgor: ZHEJIANG VEGA BIO-TECHNOLOGY CO.,LTD. Registration number: Y2022330002142 |