CN1323604C - Vine tea flavone micro capsule and its preparing method - Google Patents

Vine tea flavone micro capsule and its preparing method Download PDF

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Publication number
CN1323604C
CN1323604C CNB2005101145579A CN200510114557A CN1323604C CN 1323604 C CN1323604 C CN 1323604C CN B2005101145579 A CNB2005101145579 A CN B2005101145579A CN 200510114557 A CN200510114557 A CN 200510114557A CN 1323604 C CN1323604 C CN 1323604C
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vine tea
tea flavone
cellulose
flavone
preparation
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CN1748549A (en
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石波
梁平
王程栋
孙丽娜
李秀波
赵炳超
刘一峰
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BIOLOGY INSTITUTE GUANGXI ACADEMY OF SCIENCES
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Feed Research Institute of Chinese Academy of Agricultural Sciences
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Abstract

The present invention discloses a vine tea flavone microcapsule and a preparation method thereof. The vine tea flavone microcapsule is composed of a capsule core and capsule materials, wherein the capsule core is an extract of vine tea flavone; the capsule materials are composed of gelatin and any one kind of the following cellulose derivative which comprises ethyl cellulose, carboxymethylcellulose, phthalic acid cellulose, methyl cellulose, hypromellose, butanoic acid, cellulose acetate and succinic acid cellulose acetate. The vine tea flavone microcapsule has the advantages of high content, good fluidity and low heat loss rate. The present invention improves a biological utilization rate of the vine tea flavone as natural feed additive. Meanwhile, the present invention has the effects on promoting the growth of animals and reducing a death rate of animals.

Description

The preparation method of vine tea flavone micro capsule
Technical field
The present invention relates to the preparation method of a kind of animal, particularly a kind of preparation method of vine tea flavone micro capsule with the vine tea flavone preparation.
Background technology
Vine tea is the young stem and leaf of Vitaceae ampelopsis Ampelopsis grossedetala, has another name called sweet tea rattan.Mainly be distributed in provinces and regions such as Guangdong, Guangxi, Yunnan, Guizhou, Hunan, Hubei, Jiangxi, Fujian.Main active ingredient is flavone compound in the vine tea, and with dibydro myricetrin (being also referred to as the dihydromyricetin flavones) content for the highest.
Feed addictive is the core of mixed feed, is to improve and improve one of key of compound feed products.Development along with feed industry and herding, culture fishery, the quality of feed addictive has become the of paramount importance factor that promotes or restrict Feed Industry Development, and safety, environmentally friendly feed addictive are crucial guarantees guaranteeing human survival health.
The natural feed addictive vine tea flavone is antibiotic and active material growth promoting function of having of extracting from the porcelain ampelopsis that is rich in vine tea flavone, be mainly used in bacterial respiratory tract diseases such as treatment animal such as chicken, pig, sheep, horse, ox, can be used for promoting growth of animal simultaneously, reduce aspects such as animal dead rate.
Because oxidation inactivation, moisture absorption caking in use take place in vine tea flavone easily that extract from the porcelain ampelopsis that is rich in vine tea flavone, cause product to lose activity and add inhomogeneous, therefore for guaranteeing the reasonable utilization of vine tea flavone product, the development of carrying out vine tea flavone micro capsule has great importance.
Summary of the invention
An object of the present invention is to provide a kind of vine tea flavone micro capsule.
Vine tea flavone micro capsule provided by the present invention, form by the capsule heart and capsule material (wall material), the described capsule heart is the vine tea flavone extract, and described capsule material is gelatin and following any cellulose derivative: ethyl cellulose, carboxymethyl cellulose, O-phthalic acid cellulose, methylcellulose, Hydroxypropyl methylcellulose, cellulose acetate butyrate and butanedioic acid cellulose acetate.
Vine tea flavone extract of the present invention can extract from the old leaf of vine tea.
Described vine tea flavone extract can be the vine tea flavone powder.Contain dibydro myricetrin 92%~97% in the described vine tea flavone powder, red bayberry element (myricetin) 3%~8%; Described percentage composition is the quality percentage composition, in butt.
In the described vine tea flavone micro capsule, vine tea flavone opaque amount percentage composition is 50%-60%, and cellulose-derived amount percentage composition is 25-30%, and gelatin quality percentage composition is 11%-24%.
Described cellulose derivative is preferably ethyl cellulose.Described gelatin can be edible gelatin or pharmagel.The particle diameter of described vine tea flavone micro capsule is the 40-80 order.
Another object of the present invention provides a kind of preparation method of above-mentioned vine tea flavone micro capsule.
The preparation method of vine tea flavone micro capsule provided by the present invention, be to be the capsule heart with the vine tea flavone extract, with gelatin and following any cellulose derivative: ethyl cellulose, carboxymethyl cellulose, O-phthalic acid cellulose, methylcellulose, Hydroxypropyl methylcellulose, cellulose acetate butyrate and butanedioic acid cellulose acetate are the capsule material, by covering cohesion coating method, obtain vine tea flavone micro capsule;
Described vine tea flavone extract prepares in accordance with the following methods: the vine tea leaf is that degreasing agent carries out ungrease treatment with the organic solvent of low pole, refluxing extraction in ethanol or methyl alcohol or ethanol water or methanol aqueous solution then, centrifugal collection supernatant obtains the vine tea flavone extract.
Described degreasing agent is ether or benzinum or ethyl acetate, and consumption is 8-10 a times of described vine tea leaf quality;
The concentration of described ethanolic solution is 85%-90%, and consumption is 8-10 a times of described vine tea leaf weight.
Described vine tea flavone extract also carries out following processing: the supernatant vacuum of described centrifugal collection concentrated, and the crystallization removal of impurities, drying obtains the vine tea flavone powder;
Described ungrease treatment is for to add hot reflux 1.5-2 hour in degreasing agent; Described being extracted as in ethanol or methyl alcohol or ethanol water or methanol aqueous solution adds hot reflux 3-4 hour; Described crystallization removal of impurities is to heat 20-25 minute in 100 ℃ of boiling water baths, is cooled to room temperature.
The described cohesion coating method of covering by 6-8h, obtains vine tea flavone micro capsule at 40-60 ℃ of bag for to add vine tea flavone-cellulose derivative-carrene homogeneous phase solution in gelatin solution;
Described vine tea flavone-cellulose derivative-carrene homogeneous phase solution is prepared as follows: cellulose derivative is joined room temperature dissolving in the carrene, the cellulose derivative-dichloromethane solution that obtains; Again the vine tea flavone powder is joined in described cellulose derivative-dichloromethane solution, make vine tea flavone-ethyl cellulose-carrene homogeneous phase solution.
Described cellulose derivative is preferably ethyl cellulose; Described gelatin is edible gelatin or pharmagel.
Vine tea flavone content can reach more than 50% in the vine tea flavone micro capsule of the present invention's preparation, have content height, good fluidity, advantage that heat loss rate is low, and have slow release effect, improved the natural feed addictive vine tea flavone the biology utilization rate, avoid natural feed addictive vine tea flavone product that shortcomings such as oxidation inactivation and moisture absorption caking in use take place.The process animal is fed to test and shows that preparation of the present invention has good feeding effect, and its biology utilization rate improves 5% than the vine tea flavone product that does not wrap quilt, can obviously increase disease resistance of animals, and the feeding animals body weight is obviously increased.Vine tea flavone micro capsule production method of the present invention is simple, and package amount is big, the coating rate height, and good quality of product is easy to batch production production.
The specific embodiment
Experimental technique among the following embodiment if no special instructions, is conventional method.
Percentage composition among the following embodiment if no special instructions, is the quality percentage composition.
The preparation of embodiment 1, vine tea flavone micro capsule powder preparation
1, the preparation of vine tea flavone powder
With the ether that is 8 times of quality of the old leaf of vine tea the old leaf of vine tea is carried out ungrease treatment under the heating reflux state, the degreasing reaction time is 1.5 hours, filter then, remove organic solvent, add 90% ethanolic solution in 1: 8 ratio (ethanolic solutions of old leaf 8 weight portions of the vine tea of 1 weight portion) again, heating and refluxing extraction 4 hours, be cooled to room temperature, supernatant is collected in 3500rpm (1123g) centrifugation, 50 ℃ of following vacuum be concentrated into former supernatant volume 10% after, add the deionized water of 10 times of volumes, stir, heating is 20 minutes in 100 ℃ of boiling water baths, be cooled to room temperature, leave standstill crystalline deposit, 3500rpm (1123g) centrifugation spends deionised water, 65 ℃ of dryings 48 hours are to moisture≤8%, light green color crystalline powder vine tea flavone product.Record in this vine tea flavone dihydromyricetin flavones 95%, myricetin 4% (butt meter) by HPLC.
2, the preparation of vine tea flavone micro capsule powder
Take by weighing the 1kg edible gelatin, add 25L distilled water, the agitating heating dissolving is cooled to 50 ℃, is mixed with gelatin solution.Take by weighing the 0.75kg ethyl cellulose, add the 12.5L carrene, the stirring at room dissolving is mixed with ethyl cellulose-dichloromethane solution.Take by weighing the vine tea flavone powder of 0.55kg step 1 preparation, join in ethyl cellulose-dichloromethane solution, stir fast, make vine tea flavone-ethyl cellulose-carrene homogeneous phase solution.Add the gelatin solution that is disposed at 50L jacket type bag in by pot, maintain the temperature at 50 ℃, stir, slowly add vine tea flavone-ethyl cellulose-carrene homogeneous phase solution, stir 6h fast, cool the temperature to room temperature, behind the stirring 1h, carry out decompress filter, deionized water washing 3 times, the shape vine tea flavone micro capsule powder that must wet, 60 ℃ of dry 24h obtain 0.9kg vine tea flavone micro capsule powder product.Product yield 〉=98% (in the vine tea flavone powder), vine tea flavone content is 59.9% in the product, and the ethyl cellulose cellulose content is 25.6%, and gelatine content is 11%, and product granularity is the 40-80 order.
The preparation of embodiment 2, vine tea flavone micro capsule powder preparation
1, the preparation of vine tea flavone powder
With the benzinum that is 9 times of quality of the old leaf of vine tea the old leaf of vine tea is carried out ungrease treatment under the heating reflux state, the degreasing reaction time is 2 hours, filter then, remove organic solvent, add 85% ethanolic solution in 1: 9 ratio (ethanolic solutions of old leaf 9 weight portions of the vine tea of 1 weight portion) again, heating and refluxing extraction 3 hours, be cooled to room temperature, supernatant is collected in 3500rpm (1123g) centrifugation, 50 ℃ of following vacuum be concentrated into former supernatant volume 10% after, add the deionized water of 10 times of volumes, stir, heating is 25 minutes in 100 ℃ of boiling water baths, be cooled to room temperature, leave standstill crystalline deposit, 3500rpm (1123g) centrifugation spends deionised water, 60 ℃ of dryings 72 hours are to moisture≤8%, light green color crystalline powder vine tea flavone product.Record in this vine tea flavone dihydromyricetin flavones 92%, myricetin 6% (butt meter) by HPLC.
2, the preparation of vine tea flavone micro capsule powder
Take by weighing the 0.5kg edible gelatin, add 25L distilled water, the agitating heating dissolving is cooled to 50 ℃, is mixed with gelatin solution.Take by weighing the 0.75kg carboxymethyl cellulose, add the 12.5L carrene, stir the room temperature dissolving, be mixed with carboxymethyl cellulose-dichloromethane solution.Take by weighing the vine tea flavone powder of 0.51kg step 1, join in carboxymethyl cellulose-dichloromethane solution, stir fast, make vine tea flavone-carboxymethyl cellulose-carrene homogeneous phase solution.Add the gelatin solution that is disposed at 50L jacket type bag in by pot, maintain the temperature at 40 ℃, stir, slowly add vine tea flavone-carboxymethyl cellulose-carrene homogeneous phase solution, stir 7h fast, cool the temperature to room temperature, behind the stirring 1h, carry out decompress filter, deionized water washing 3 times, the shape vine tea flavone micro capsule powder that must wet, 65 ℃ of dry 24h obtain 1.0kg vine tea flavone micro capsule powder product.Product yield 〉=98% (in the vine tea flavone powder), vine tea flavone content is 50% in the product, and carboxymethyl cellulose level is 27%, and gelatine content is 18%, and product cut size is the 40-80 order.
The preparation of embodiment 3, vine tea flavone micro capsule powder preparation
1, the preparation of vine tea flavone powder
With the ethyl acetate that is 10 times of quality of the old leaf of vine tea the old leaf of vine tea is carried out ungrease treatment under the heating reflux state, the degreasing reaction time is 1.8 hours, filter then, remove organic solvent, add 90% methanol solution in 1: 8 ratio (methanol solutions of old leaf 8 weight portions of the vine tea of 1 weight portion) again, heating and refluxing extraction 3.5 hours, be cooled to room temperature, supernatant is collected in 3500rpm (1123g) centrifugation, 50 ℃ of following vacuum be concentrated into former supernatant volume 10% after, add the deionized water of 10 times of volumes, stir, heating is 23 minutes in 100 ℃ of boiling water baths, be cooled to room temperature, leave standstill crystalline deposit, 3500rpm (1123g) centrifugation spends deionised water, 63 ℃ of dryings 50 hours are to moisture≤8%, light green color crystalline powder vine tea flavone product.Record in this vine tea flavone dihydromyricetin flavones 96%, myricetin 3% (butt meter) by HPLC.
2, the preparation of vine tea flavone micro capsule powder
Take by weighing the 1.0kg edible gelatin, add 25L distilled water, the agitating heating dissolving is cooled to 45 ℃, is mixed with gelatin solution.Take by weighing the 1.0kg methylcellulose, add the 12.5L carrene, stir the room temperature dissolving, be mixed with methylcellulose-dichloromethane solution.Take by weighing the vine tea flavone powder of 0.51kg step 1, join in methylcellulose-dichloromethane solution, stir fast, make vine tea flavone-methylcellulose-carrene homogeneous phase solution.Add the gelatin solution that is disposed at 50L jacket type bag in by pot, maintain the temperature at 60 ℃, stir, slowly add vine tea flavone-methylcellulose-carrene homogeneous phase solution, stir 8h fast, cool the temperature to room temperature, behind the stirring 1h, carry out decompress filter, distilled water washing 3 times, the shape vine tea flavone micro capsule powder that must wet, 60 ℃ of dry 24h obtain 0.95kg vine tea flavone micro capsule powder product.Product yield 〉=98% (in the vine tea flavone powder), vine tea flavone content is 52.6% in the product, and methylcellulose content is 25%, and gelatine content is 16.4%, and product cut size is the 40-80 order.

Claims (6)

1, the preparation method of vine tea flavone micro capsule may further comprise the steps:
1) with vine tea leaf quality 8-10 ether or benzinum or ethyl acetate doubly the vine tea leaf is carried out ungrease treatment;
2) the vine tea leaf after the degreasing is the ethanolic solution refluxing extraction of 85%-90% with its quality 8-10 concentration doubly, and centrifugal collection supernatant obtains the vine tea flavone extract;
3) the supernatant vacuum with described centrifugal collection concentrates, the crystallization removal of impurities, and drying obtains the vine tea flavone powder;
4) be the capsule heart with the vine tea flavone powder, with gelatin and following any cellulose derivative: ethyl cellulose, carboxymethyl cellulose, O-phthalic acid cellulose, methylcellulose, Hydroxypropyl methylcellulose, cellulose acetate butyrate and butanedioic acid cellulose acetate are the capsule material, by covering cohesion coating method, obtain vine tea flavone micro capsule;
Wherein, in the described vine tea flavone micro capsule, vine tea flavone opaque amount percentage composition is 50%-60%, and cellulose-derived amount percentage composition is 25-30%, and gelatin quality percentage composition is 11%-24%; The described cohesion coating method of covering by 6-8h, obtains vine tea flavone micro capsule at 40-60 ℃ of bag for to add vine tea flavone-cellulose derivative-carrene homogeneous phase solution in gelatin solution.
2, preparation method according to claim 1 is characterized in that: described ungrease treatment is for to add hot reflux 1.5-2 hour in degreasing agent.
3, preparation method according to claim 1 and 2 is characterized in that: the time of described refluxing extraction is 3-4 hour.
4, preparation method according to claim 1 and 2 is characterized in that: described crystallization removal of impurities is to heat 20-25 minute in 100 ℃ of boiling water baths, is cooled to room temperature.
5, preparation method according to claim 1 and 2, it is characterized in that: described vine tea flavone-cellulose derivative-carrene homogeneous phase solution is prepared as follows: cellulose derivative is joined room temperature dissolving in the carrene, the cellulose derivative-dichloromethane solution that obtains; Again the vine tea flavone powder is joined in described cellulose derivative-dichloromethane solution, make vine tea flavone-ethyl cellulose-carrene homogeneous phase solution.
6, preparation method according to claim 1 and 2 is characterized in that: described cellulose derivative is an ethyl cellulose; Described gelatin is edible gelatin or pharmagel.
CNB2005101145579A 2005-10-26 2005-10-26 Vine tea flavone micro capsule and its preparing method Active CN1323604C (en)

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Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101810735B (en) * 2010-04-16 2012-01-11 安徽省瑞森生物科技有限责任公司 Method for extracting total flavone from ampelopsis grossedentata
CN103168916A (en) * 2012-06-12 2013-06-26 北京伟嘉人生物技术有限公司 Animal health-care feed
CN102885177A (en) * 2012-10-25 2013-01-23 安吉依思味食品有限公司 An Ji white tea micro-capsule and preparation method thereof
CN103127198B (en) * 2013-03-01 2015-01-21 成都乾坤动物药业有限公司 Combined drug for treating piglet's yellow-white dysentery
CN103431185B (en) * 2013-09-10 2014-12-17 湖南大北农农业科技有限公司 Livestock feed and preparation method thereof
CN104026349A (en) * 2014-06-05 2014-09-10 江口县致远生产力促进中心 Feed additive as well as preparation method and application thereof
CN104472876A (en) * 2014-12-10 2015-04-01 张家界恒兴生物科技有限公司 Production method of special plant feed additive for aquaculture
CN108478538A (en) * 2018-04-12 2018-09-04 铜仁学院 A kind of preparation process of dihydromyricetin from Ampelopsis grossedentata capsule
CN110122693A (en) * 2019-05-28 2019-08-16 常熟市金牧药业有限公司 Pig compound premix
CN115944082A (en) * 2023-01-03 2023-04-11 时代生物科技(深圳)有限公司 Whitening anti-saccharification composition and preparation method thereof

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