CN1380056A - Preparation method of high-content oil-soluble vitamin slow-releasing microcapsule powder - Google Patents
Preparation method of high-content oil-soluble vitamin slow-releasing microcapsule powder Download PDFInfo
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- CN1380056A CN1380056A CN 01107337 CN01107337A CN1380056A CN 1380056 A CN1380056 A CN 1380056A CN 01107337 CN01107337 CN 01107337 CN 01107337 A CN01107337 A CN 01107337A CN 1380056 A CN1380056 A CN 1380056A
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Abstract
The preparation method of high content oil-soluble liquid vitamin slow release microcapsule powder is characterized by that it adopts an 0 O1/W/O2 compound emulsion coating process, it can make one or several emulsion particles be coated in one capsule-shaped external shell, so that in the course of replease said microcapsule can release oil particles one-by-one so as to attain the effect of long-acting slow-release. Its vitamin conten can be up to above 70%, it can be made into tablet, and possesses good slow release effect.
Description
The invention relates to a kind of preparation method of high-content oil-soluble liquid vitamins slow-releasing microcapsule powder.The oil soluble liquid vitamins comprises the succinate of the acetate of vitamin E or vitamin A or vitamin E or A or vitamin E or dissolves in the oil-soluble solid vitamin of oiliness material such as the mixture of vitamin D or vitamin K or two or more fat soluble vitamin etc., belongs to biomedical sector.
Oil soluble liquid vitamins product such as vitamin E (being called for short VE), since finding, it enlarges day by day at medical industry and Application in Food Industry.Nineteen fifty-nine, U.S. food and the official confirmation VE of nutrition committee are the essential compositions of human nutrition.Because VE has many physiological functions, so FAO (Food and Agriculture Organization of the United Nation) and World Health Organization's suggestion replenish an amount of VE to satisfy human body requirements every day.The major function of VE is: (1) antisterility function can be used for treating habituation or threatened abortion; (2) antitumaous effect; (3) can be used for treating cardiovascular disease such as coronary heart disease, myocardial infarction, arteriosclerosis; (4) have anti-oxidation function, and can improve the utilization rate of oxygen in the blood, thereby improve muscle endurance, can be used for treatment of diseases such as progressive muscular dystrophy; (5) have anti-aging effects, can strengthen the human body immune function, the old people takes VE for a long time, can improve its general situation, comprises the functional status of lymphsystem, skeletal muscle and cardiovascular system.In order to make full use of these functions of VE, various forms of VE new product technologies of preparing continue to bring out, thereby it is more widely used at aspects such as medicines and health protection, food industry, cosmetics industry, animal feed and sensitive materials.But along with the increase of oral VE number, the especially increase of the oral quantity of old people, present dosage form just seems and is far from suitable.Because peroral dosage form still based on capsule, is the assurance high-load, efficient, capsule is done bigger and bigger.But after this capsule enters human body, a large amount of contents still exist with the grease form, thereby, there is major defect aspect flowability, the absorption, show as low bioavailability, therefore study VE new product and just seem extremely important with high bioactivity and high-absorbility.
The main component of VE is an alpha-tocopherol, but normally oil-soluble liquid such as tocopherol and ester type compound thereof such as tocopherol acetate, tocopherol succinate etc., and water insoluble, its bioavailability is low, and absorption difference uses and transports also extremely inconvenient.For improving bioavailability and absorption efficiency, to be convenient to again take, pack, transport and sell, exploitation VE powder or VE sustained-release micro-spheres powder have become the developing direction of this product.At present, the domestic common VE powder (content: 50%), be mainly used in animal feed additive of only producing.And abroad, pharmaceutical grade high-load VE sustained-release micro-spheres powder (content: 75%) except that as the medical product, also be widely used as nutrient additive for food and food supplement, improved the bioavailability of VE greatly, also opened up new wide market for the application of VE powder.
United States Patent (USP) (6,030,645) introduced a kind of method for preparing the oil soluble liquid microcapsule, be that oil soluble material emulsifyings such as VE are dispersed in the aqueous gelatin solution, form minuteness particle, by spray drying, emulsion is sprayed on the bed that is paved with the calcium silicates powder, form the microcapsule that the outside is surrounded by calcium silicate powder.
The high-load VE powder of preparation that United States Patent (USP) (6,020,003) is introduced is to make the capsule material with a kind of not gelatin hydrolysate, and VE emulsifying is dispersed in the aqueous gelatin solution, forms minuteness particle, makes by spray drying.
United States Patent (USP) (6,001,554) method for preparing high-load VE microcapsule of Jie Shaoing is by VE emulsifying being dispersed in the aqueous solution of cellulose ether, by changing temperature or regulating pH, make the capsule material solidify to form primary particle, the aqueous solution that adds another seed capsules material again carries out coating the second time or coating for the third time, and the particle of Xing Chenging makes microcapsule by spray drying at last.
There is following technical deficiency in above-mentioned technology: only by spray drying granulation, the difficult control of balling-up size coats also tightly inadequately, makes olefiant seepage easily, does not have slow releasing function; On the other hand, repeatedly coating is difficult to accomplish high oil content.
The preparation method that the objective of the invention is to avoid deficiency of the prior art and a kind of high-content oil-soluble liquid vitamins slow-releasing microcapsule powder is provided.A kind of preparation method of high-content oil-soluble liquid vitamins slow-releasing microcapsule powder, its characteristics are to adopt Water-In-Oil bag oil (O
1/ W/O
2) the emulsion cladding process, the vitamin slow-releasing microcapsule powder of preparation can form nucleocapsid structure, and one or more emulsion particles are covered by in the scrotiform shell, and the microcapsule of Xing Chenging is in dispose procedure like this, can one by one elaioleucite be discharged, reach the effect of long-acting slow-release.Adopt the vitamins slow-releasing microcapsule powder vitamin content of the present invention's preparation can reach more than 70%, have the feature of content height, good fluidity, anti-extruding, can further make tablet, have good slow release effect.
Purpose of the present invention can reach by following measure: the plain analog derivative of the outer clad material series fiber of high-load vitamin slow-releasing microcapsule powder or polypeptide class such as Biodegradable materials such as gelatin or polysaccharide such as arabic gum account for the 8-15%wt of microcapsule; Comprised the succinate of the acetate of vitamin E or vitamin A or vitamin E or A or vitamin E or dissolve in the oil-soluble solid vitamin of oiliness material such as the mixture of vitamin D or vitamin K or two or more fat soluble vitamin etc. that the content of oil soluble materials such as the vitamin that is coated or its ester is more than 70% by the oil soluble liquid vitamins that coated; The center of high-load vitamin slow-releasing microcapsule is the O/w emulsion kernel, includes one or more emulsion particles; The particle diameter of high-load vitamin slow-releasing microcapsule is at 100-400 μ m.The microcapsule clad material is cellulose derivative such as biodegradable hydroxypropyl cellulose, hydroxypropyl emthylcellulose, hydroxypropylmethyl cellulose phthalate, ethyl cellulose, methylcellulose etc. or polypeptide analog derivative such as biomedical materials such as polyamino acid, gelatin etc. or polysaccharide derivatives such as arabic gum, sodium alginate.Can be wherein a kind of, also can be two or more mixtures of material.For fat soluble vitamin is the microcapsule of capsule core material, adopts Water-In-Oil bag oil (O
1/ W/O
2) the oil bath seasoning, earlier vitamin is adsorbed on a kind of efficient oil-absorbing carrier material, will adsorb greasy carrier and oils and fats (O again
1) be dispersed in and form oil-in-water system (O in a kind of heavy-gravity aqueous capsule material solution (w)
1/ W), allow oils and fats form microsphere, the carrier subparticle disperses therebetween, makes trickle carrier granular accumulate in microsphere surface by emulsification again.Wherein water (w) and oil phase (O
1) volume ratio be 2-10: 1, used its HLB value (hydrophile-lipophile balance value) of emulsifying agent of water is more than 10, consumption is the 0.1%-10%wt of water; Again this oil-in-water system is dispersed in another organic solvent phase (O
2) in, by emulsification, form stable Water-In-Oil bag oil (O
1/ W/O
2) system, the oil phase (O of its China and foreign countries
2) with internal layer oil-in-water (O mutually
1/ W) volume ratio is 2-100: 1, and its HLB value of the used emulsifying agent of outer oil phase is below 10, and consumption is outer oil phase (O
2) 0.1%-10%wt; Last pH by the change system again or reduce temperature to reduce the dissolubility of water-soluble polymer makes the waterborne polymeric that has wrapped up the fat soluble vitamin microsphere tentatively fixing, or passes through crosslinking curing, again spray drying or be dried into exsiccant microsphere.Adopt the oil bath seasoning of Water-In-Oil bag oil, used outer oil phase comprises the mixed solvent of liquid paraffin, Oleum Glycines, Semen Allii Tuberosi wet goods oil solvent or itself and organic solvent such as dichloromethane, cyclohexane extraction, ethyl acetate.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1, the 10g gelatin is dissolved in 150 ml distilled waters, add in the there-necked flask, constant speed stirs 20min under 500rpm, the sodium lauryl sulphate of adding 1%, after dispersed with stirring is even, the powder mixes of 65g vitamin E and 3g silicon dioxide is joined above-mentioned aqueous phase after evenly, form oil-in-water system (O
1/ W), emulsifying is 1 hour under 40 ℃ of stirrings, then this system is poured in about 300 milliliters of isothermal liquid paraffin that contain 3 milliliters of department classes 80, and 400rpm stirs 30min, and being emulsified into Water-In-Oil bag oil body is (O
1/ W/O
2), treat when becoming grain diameter to meet the requirements, system is reduced to below 5 ℃, formaldehyde solidified 2 hours, the solid microcapsule.System is poured out centrifugal, the oven dry, promptly get the drying solid microcapsule.The content of the vitamin E of gained microcapsule is near 80%.
Embodiment 2, the 10g gelatin is dissolved in 200 ml distilled waters, add in the there-necked flask, constant speed stirs 20min under 500rpm, the sodium lauryl sulphate of adding 0.5%, after dispersed with stirring is even, the pressed powder 50g of vitamin D is become paste with 10ml Oleum Glycines stirring and evenly mixing, add and pour in the aqueous gelatin solution after the 10-15ml ethyl acetate is diluted, form oil-in-water system (O
1/ W), emulsifying is 1 hour under 75 ℃ of stirrings, treats after ethyl acetate is waved to the greatest extent this system to be poured in about 400 milliliters of isothermal liquid paraffin that contain 4 milliliters of classes of department 80, and 400rpm stirs 30min, and being emulsified into Water-In-Oil bag oil body is (O
1/ W/O
2), treat when becoming grain diameter to meet the requirements, system is reduced to below 5 ℃, formaldehyde solidified 2 hours, the solid microcapsule.System is poured out centrifugal, after the washed with isopropyl alcohol, the oven dry, promptly get the drying solid microcapsule.The content of the vitamin D of gained microcapsule is near 85%.
Embodiment 3, the 10g gelatin is dissolved in 200 ml distilled waters, add in the there-necked flask, constant speed stirs 20min under 500rpm, the sodium lauryl sulphate of adding 1.5%, after dispersed with stirring is even, with the oily mixture of 65g vitamin E and vitamin A (1: 1v/v) join above-mentioned aqueous phase after evenly, form oil-in-water system (O with the powder mixes of 5g silicon dioxide
1/ W), emulsifying is 1 hour under 40 ℃ of stirrings, then this system is poured in about 800 milliliters of isothermal liquid paraffin that contain 3 milliliters of department classes 80, and 400rpm stirs 30min, and being emulsified into Water-In-Oil bag oil body is (O
1/ W/O
2), treat when becoming grain diameter to meet the requirements, system is reduced to below 5 ℃, formaldehyde solidified 2 hours, the solid microcapsule.System is poured out centrifugal, the oven dry, promptly get the drying solid microcapsule.The content of the vitamin ae microcapsule of gained microcapsule is near 75%.The more traditional vitamin ae soft gelatin capsule of this kind vitamin ae microcapsule has tangible slow releasing function.
Claims (6)
1, a kind of preparation method of high-content oil-soluble liquid vitamins slow-releasing microcapsule powder is characterized in that adopting Water-In-Oil bag oil (O
1/ W/O
2) the emulsion cladding process; The vitamin slow-releasing microcapsule powder of preparation can form nucleocapsid structure, one or more emulsion particles are covered by in the scrotiform shell, plain analog derivative of the outer clad material series fiber of high-load vitamin slow-releasing microsphere powder or Biodegradable materials such as polypeptide analog derivative or polysaccharide derivatives account for the 8-15%wt of microcapsule; The core-clad material that is coated is an oil soluble liquid vitamins product, and the content of the fat soluble vitamin that is coated is more than 70%; The center of high-load vitamin slow-releasing microcapsule is exsiccant O/w emulsion kernel, includes one or more emulsion particles; The particle diameter of high-load vitamin slow-releasing microcapsule is at 100-400 μ m, and the vitamins slow-releasing microcapsule powder of preparation has the feature of content height, good fluidity, anti-extruding, can further make tablet.
2, high-content oil-soluble liquid vitamin microcapsule powder as claimed in claim 1 is characterized in that the microcapsule clad material is cellulose derivative such as biodegradable hydroxypropyl cellulose, hydroxypropyl emthylcellulose, hydroxypropylmethyl cellulose phthalate, ethyl cellulose, methylcellulose etc.; Or polypeptide analog derivative such as polyamino acid, gelatin etc.; Or biomedical materials such as polysaccharide derivatives such as arabic gum, sodium alginate; Can be wherein a kind of, also can be two or more mixtures of material.
3, the core-clad material that is coated as claimed in claim 1 is an oil soluble liquid vitamins product, it is characterized in that oil soluble liquid vitamins product comprises the succinate of the acetate of vitamin E or vitamin A or vitamin E or A or vitamin E or is dissolved in the oil-soluble solid vitamin of oily matter such as the mixture of vitamin D or vitamin K or two or more fat soluble vitamin etc.
4, the preparation method of microcapsule powder as claimed in claim 1 is characterized in that for fat soluble vitamin being the microcapsule of capsule core material, adopts Water-In-Oil bag oil (O
1/ W/O
2) the oil bath seasoning, earlier vitamin is adsorbed on a kind of efficient oil-absorbing carrier material, will adsorb greasy carrier and oils and fats (O again
1) be dispersed in and form oil-in-water system (O in a kind of heavy-gravity aqueous capsule material solution (w)
1/ W), allow oils and fats form microsphere, the carrier subparticle disperses therebetween, makes trickle carrier granular accumulate in microsphere surface by emulsification again, wherein water (w) and oil phase (O
1) volume ratio be 2-10: 1, used its HLB value (hydrophile-lipophile balance value) of emulsifying agent of water is more than 10, consumption is the 0.1%-10%wt of water; Again this oil-in-water system is dispersed in another organic solvent phase (O
2) also claim by emulsification, to form stable Water-In-Oil bag oil (O in the outer oil phase
1/ W/O
2) system, the oil phase (O of its China and foreign countries
2) with internal layer oil-in-water (O mutually
1/ W) volume ratio is 2-100: 1, and its HLB value of the used emulsifying agent of outer oil phase is below 10, and consumption is outer oil phase (O
2) 0.1%-10%wt; Last pH by the change system again or reduce temperature to reduce the dissolubility of water-soluble polymer makes the waterborne polymeric that has wrapped up the fat soluble vitamin microsphere tentatively fixing, or passes through crosslinking curing, again spray drying or be dried into exsiccant microsphere.
5, the efficient oil-absorbing carrier material as being adopted in the claim 4 is characterized in that it can being inert materials such as Pulvis Talci, silicon dioxide, calcium silicates, Kaolin.
6, the preparation method of the high-content oil-soluble liquid vitamin slow-releasing microcapsule described in claim 4 is characterized in that used outer oil phase comprises the mixed solvent of liquid paraffin, Oleum Glycines, Semen Allii Tuberosi wet goods oil solvent or itself and organic solvent such as dichloromethane, cyclohexane extraction, ethyl acetate.
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|---|---|---|---|
| CN 01107337 CN1203843C (en) | 2001-04-10 | 2001-04-10 | Preparation method of high-content oil-soluble vitamin slow-releasing microcapsule powder |
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|---|---|---|---|
| CN 01107337 CN1203843C (en) | 2001-04-10 | 2001-04-10 | Preparation method of high-content oil-soluble vitamin slow-releasing microcapsule powder |
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| CN1380056A true CN1380056A (en) | 2002-11-20 |
| CN1203843C CN1203843C (en) | 2005-06-01 |
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Cited By (17)
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|---|---|---|---|---|
| CN1314453C (en) * | 2003-09-25 | 2007-05-09 | 中国科学院过程工程研究所 | Stable stored composite emulsion carrier in even dimension for hydrophilicity medication and preparation method |
| CN100348181C (en) * | 2005-09-28 | 2007-11-14 | 浙江大学 | Water-dispersive nano-grade ibuprofen injecta and preparing method |
| CN100358511C (en) * | 2005-09-28 | 2008-01-02 | 浙江大学 | Oil-soluble medicine degradable polymer microcapsule injecta and preparing method |
| CN1927188B (en) * | 2006-08-25 | 2010-10-06 | 西南合成制药股份有限公司 | Voltage endurance vitamin E microcapsule and its preparing process |
| CN101953817A (en) * | 2010-09-20 | 2011-01-26 | 同济大学 | Microcapsules with oil-soluble substances and preparation method thereof |
| CN102580638A (en) * | 2012-03-13 | 2012-07-18 | 江南大学 | Microencapsulation method for preparing hydrotropic substance serving as core material by using complex coacervation method |
| CN103392757A (en) * | 2013-06-30 | 2013-11-20 | 安徽省凤宝粮油食品（集团）有限公司 | Microcapsule nutritious flour improver |
| CN103534343A (en) * | 2011-02-14 | 2014-01-22 | 诺丁汉大学 | Oil body extraction and uses |
| CN105213318A (en) * | 2009-05-18 | 2016-01-06 | 希格默伊德药业有限公司 | Comprise the compositions of oil droplet |
| CN106213308A (en) * | 2016-08-04 | 2016-12-14 | 务川茂源现代农业开发有限公司 | Formula of Rhizoma amorphophalli nutritive powder and preparation method thereof |
| CN107875139A (en) * | 2017-10-09 | 2018-04-06 | 中山大学 | A kind of shell core alpha tocopherol microcapsules and preparation method thereof |
| CN103874422B (en) * | 2011-10-14 | 2018-05-11 | 帝斯曼知识产权资产管理有限公司 | Coat system |
| CN108208838A (en) * | 2018-03-09 | 2018-06-29 | 北京素维生物科技有限公司 | A kind of taste masking composition and application thereof |
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| CN110974719A (en) * | 2019-12-26 | 2020-04-10 | 东莞波顿香料有限公司 | Vitamin E sustained-release granules, preparation method thereof and washing and caring product |
| CN112107555A (en) * | 2020-09-18 | 2020-12-22 | 万华化学集团股份有限公司 | Vitamin A acetate microcapsule and preparation method thereof |
| CN112544970A (en) * | 2020-12-11 | 2021-03-26 | 江南大学 | Preparation method of starch-based double emulsion embedded with fat-soluble functional factors |
-
2001
- 2001-04-10 CN CN 01107337 patent/CN1203843C/en not_active Expired - Fee Related
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1314453C (en) * | 2003-09-25 | 2007-05-09 | 中国科学院过程工程研究所 | Stable stored composite emulsion carrier in even dimension for hydrophilicity medication and preparation method |
| CN100348181C (en) * | 2005-09-28 | 2007-11-14 | 浙江大学 | Water-dispersive nano-grade ibuprofen injecta and preparing method |
| CN100358511C (en) * | 2005-09-28 | 2008-01-02 | 浙江大学 | Oil-soluble medicine degradable polymer microcapsule injecta and preparing method |
| CN1927188B (en) * | 2006-08-25 | 2010-10-06 | 西南合成制药股份有限公司 | Voltage endurance vitamin E microcapsule and its preparing process |
| CN105213318A (en) * | 2009-05-18 | 2016-01-06 | 希格默伊德药业有限公司 | Comprise the compositions of oil droplet |
| CN101953817B (en) * | 2010-09-20 | 2011-12-07 | 同济大学 | Microcapsules with oil-soluble substances and preparation method thereof |
| CN101953817A (en) * | 2010-09-20 | 2011-01-26 | 同济大学 | Microcapsules with oil-soluble substances and preparation method thereof |
| CN103534343A (en) * | 2011-02-14 | 2014-01-22 | 诺丁汉大学 | Oil body extraction and uses |
| CN103874422B (en) * | 2011-10-14 | 2018-05-11 | 帝斯曼知识产权资产管理有限公司 | Coat system |
| CN102580638A (en) * | 2012-03-13 | 2012-07-18 | 江南大学 | Microencapsulation method for preparing hydrotropic substance serving as core material by using complex coacervation method |
| CN103392757A (en) * | 2013-06-30 | 2013-11-20 | 安徽省凤宝粮油食品（集团）有限公司 | Microcapsule nutritious flour improver |
| CN103392757B (en) * | 2013-06-30 | 2015-06-17 | 安徽省凤宝粮油食品（集团）有限公司 | Microcapsule nutritious flour improver |
| CN106213308A (en) * | 2016-08-04 | 2016-12-14 | 务川茂源现代农业开发有限公司 | Formula of Rhizoma amorphophalli nutritive powder and preparation method thereof |
| CN107875139A (en) * | 2017-10-09 | 2018-04-06 | 中山大学 | A kind of shell core alpha tocopherol microcapsules and preparation method thereof |
| CN108208838A (en) * | 2018-03-09 | 2018-06-29 | 北京素维生物科技有限公司 | A kind of taste masking composition and application thereof |
| CN110917071A (en) * | 2019-12-23 | 2020-03-27 | 上海万华科聚化工科技发展有限公司 | Core-shell structure flexible bead, preparation method thereof and personal care product comprising core-shell structure flexible bead |
| CN110917071B (en) * | 2019-12-23 | 2022-11-08 | 万华化学集团股份有限公司 | Core-shell structure flexible bead, preparation method thereof and personal care product comprising core-shell structure flexible bead |
| CN110974719A (en) * | 2019-12-26 | 2020-04-10 | 东莞波顿香料有限公司 | Vitamin E sustained-release granules, preparation method thereof and washing and caring product |
| CN112107555A (en) * | 2020-09-18 | 2020-12-22 | 万华化学集团股份有限公司 | Vitamin A acetate microcapsule and preparation method thereof |
| CN112107555B (en) * | 2020-09-18 | 2023-03-17 | 万华化学集团股份有限公司 | Vitamin A acetate microcapsule and preparation method thereof |
| CN112544970A (en) * | 2020-12-11 | 2021-03-26 | 江南大学 | Preparation method of starch-based double emulsion embedded with fat-soluble functional factors |
| WO2022121133A1 (en) * | 2020-12-11 | 2022-06-16 | 江南大学 | Preparation method for fat-soluble functional factor-embedded starch-based double emulsion |
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