CN1927188A - Voltage endurance vitamin E microcapsule and its preparing process - Google Patents

Voltage endurance vitamin E microcapsule and its preparing process Download PDF

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Publication number
CN1927188A
CN1927188A CNA2006100950692A CN200610095069A CN1927188A CN 1927188 A CN1927188 A CN 1927188A CN A2006100950692 A CNA2006100950692 A CN A2006100950692A CN 200610095069 A CN200610095069 A CN 200610095069A CN 1927188 A CN1927188 A CN 1927188A
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China
Prior art keywords
vitamin
component
microcapsule
voltage endurance
octenyl succinate
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CNA2006100950692A
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Chinese (zh)
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CN1927188B (en
Inventor
赵洪武
王海屿
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PKU HEALTHCARE CORP., LTD.
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Southwest Synthetic Pharmaceutical Corp Ltd
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Abstract

The invention relates to pressure resistant vitamin E capsules, wherein the constituents include (by weight percent) vitamin E oil 50-70%, capsule material 1-25%, auxiliary capsule material 5-30%, octenylsuccinate starch 10-30%, flow aid 0.5-2%. The invention also relates to the process for preparing the capsules.

Description

A kind of voltage endurance vitamin E microcapsule and preparation method thereof
Technical field
The present invention relates to a kind of voltage endurance vitamin E microcapsule and preparation method thereof.
Technical background
Vitamin E has another name called tocopherol, runs concurrently for a kind of common drug and supports health product, has become maximum, the great main vitamins kind of volume of production and marketing of purposes on the international market at present.The most outstanding chemical property of vitamin E is an antioxidation, and it can strengthen the antioxidation of cell, has to utilize the integrity of keeping various cell membrane; Participate in many-sided metabolic process of some whole cell tissue; Effects such as the vigor of maintenance membrane bound enzyme and receptor; In addition it also have anti-aging effects, blood coagulation resisting function, enhancing immunity, improvement end slightly blood circulation, prevent arteriosclerosis, keep erythrocyte, leukocyte, brain cell, epithelial integrity, thus the normal function of maintenance muscle, neural blood vessel and hemopoietic system etc.
Be golden yellow or faint yellow thickness oily liquids under the vitamin E room temperature, transportation and use metering are inconvenient, and because of its oxidisability instability, having developed content inside and outside the native land one after another is 20%~70% vitamin E microcapsule powder, but when it directly applies to tablet, the easily broken capsule because the mechanical strength of its capsule is not high, content step-down during stability study shows vitamin E oxidation deterioration behind its broken capsule.
Summary of the invention
Technical problem to be solved by this invention provides a kind of voltage endurance vitamin E microcapsule and preparation method thereof, by with common emulsifying such as vitamin E oil, mictocystis material, fluidizer, homogenizing, spray drying is made the mobile powder of microencapsulation, can be dispersed in the cold water, the significant mechanical strength that improves microcapsule of new prescription can be directly used in tabletting, and this product can be used in medicine and the food.
The composition of the voltage endurance vitamin E microcapsule that the present invention relates to is such: the percentage by weight between its component and the component is: vitamin E oil 50%~70%, capsule material 1%~25%, auxiliary capsule material 5%~30%, octenyl succinate starch 10%~30%, fluidizer 0.5%~2%.
In the said components of the present invention:
1, vitamin E is a Main Ingredients and Appearance, the vitamin E powder of selling on the market mostly is greatly and contains vitamin E 50%~70%, vitamin E powder integrated cost in this content range is lower, and the later stage uses interpolation also comparatively convenient, contains vitamin E 50%~70% so vitamin E microcapsule of the present invention also is decided to be.
2, gelatin is the capsule material, a kind of in also available arabic gum, alginate, chitosan, the casein or more than 2 kinds.
3, dextrin prevents microcapsule adhesion in the spray-drying process for auxiliary capsule material, and available lactose, mannitol, sorbitol etc. are a kind of or more than 2 kinds.
4, octenyl succinate starch is the good emulsifying agent capsule material of holding concurrently, and can greatly strengthen the mechanical strength of microcapsule.
5, micropowder silica gel is a fluidizer, a kind of or mixing replacement more than 2 kinds such as available Pulvis Talci, magnesium stearate.The capsule material is selected: it is main capsule material that novel capsule material octenyl succinate starch is selected in this experiment for use, add a small amount of high score ascus material, the auxiliary capsule material of dextrin class and fluidizer, the emulsifying spray drying forms, select different prescriptions for use according to different oil content, optimize capsule material proportioning: octenyl succinate starch: high score ascus material: the dextrin class is assisted capsule material=(35~40): (5~10): (10~22).
Preparation method:
1), preparation aqueous phase solution: 1~3 times the purified water of always measuring admittedly by above-mentioned microcapsule component is heated to 65~70 ℃, by proportioning capsule material, octenyl succinate starch, auxiliary capsule material and fluidizer is slowly added, and stirs it to be uniformly dispersed in 8~15 minutes.
2), preparation oil phase liquid: vitamin E oil is preheated to 65~70 ℃ by proportioning.
3), the emulsifying homogenizing: above-mentioned fluid is slowly added aqueous phase solution mutually, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, getting emulsion examines under a microscope, answer encapsulation complete and big or small about 10 μ m, as do not reach requirement, homogenizing is observed again;
4), spray drying: above-mentioned emulsion is added in the centrifugal spray dryer, is 180 ℃~190 ℃ in inlet temperature, 85~90 ℃ of air-out, the centrifugal energy nozzle rotating speed is under 20,000~30,000 conditions of changeing, and carries out spray drying;
5), check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
The voltage endurance vitamin E microcapsule outward appearance that makes is pure white, and flowability and compressibility are good, adds conventional adjuvant and can carry out tabletting or filled capsules.This product also has good water dispersible, can disperse rapidly at cold water, can be as the additive of food such as beverage, ice river in Henan Province icepro, cake and confection class in food.
The present invention is on old technology basis, adding novel adjuvant octenyl succinate starch forms through emulsifying, homogenizing, spray drying, the new octenyl succinate starch that adds has first-class film property and good emulsibility, can improve the mechanical strength of microcapsule greatly, be enough to satisfy the tabletting requirement, and fuel load can be up to 70%, encapsulation rate height, good fluidity.
The specific embodiment
Embodiment 1:
Vitamin E 50%
Gelatin 5%
Dextrin 12%
Octenyl succinate starch 32%
Micropowder silica gel 1%
Purified water is 1.5 times of weight of solid amount always
Preparation method:
1, water: the purified water of recipe quantity is heated to 65~70 ℃, gelatin, octenyl succinate starch, dextrin and the micropowder silica gel of recipe quantity slowly added, stir and it was uniformly dispersed in 10 minutes.
2, oil phase: the vitamin E oil of recipe quantity is preheated to 65~70 ℃.
3, emulsifying homogenizing: oil phase is slowly added water, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, gets emulsion and examines under a microscope, and answers encapsulation complete and big or small about 10 μ m, as does not reach requirement, and homogenizing is observed again.
4, spray drying: emulsion is added in the centrifugal spray dryer, and inlet temperature is 180 ℃~190 ℃, 85~90 ℃ of air-out, and the centrifugal energy nozzle rotating speed is 20,000~30,000 commentaries on classics, opens Liquid spraying pump and carries out spray drying.
5, check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
Embodiment 2
Vitamin E 55%
Sodium caseinate 9%
Lactose 10%
Octenyl succinate starch 25%
Micropowder silica gel 1%
Purified water is 1.5 times of weight of solid amount always
Preparation method:
1, water: the purified water of recipe quantity is heated to 65~70 ℃, sodium caseinate, octenyl succinate starch, lactose and the micropowder silica gel of recipe quantity slowly added, stir and it was uniformly dispersed in 10 minutes.
2, oil phase: the vitamin E oil of recipe quantity is preheated to 65~70 ℃.
3, emulsifying homogenizing: oil phase is slowly added water, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, gets emulsion and examines under a microscope, and answers encapsulation complete and big or small about 10 μ m, as does not reach requirement, and homogenizing is observed again.
4, spray drying: emulsion is added in the centrifugal spray dryer, and inlet temperature is 180 ℃~190 ℃, 85~90 ℃ of air-out, and the centrifugal energy nozzle rotating speed is 20,000~30,000 commentaries on classics, opens Liquid spraying pump and carries out spray drying.
5, check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
Embodiment 3
Vitamin E 60%
Chitosan 6%
Lactose 12%
Octenyl succinate starch 20.8%
Micropowder silica gel 1.2%
Purified water is 1.5 times of weight of solid amount always
Preparation method:
1, water: the purified water of recipe quantity is heated to 65~70 ℃, chitosan, octenyl succinate starch, lactose and the micropowder silica gel of recipe quantity slowly added, stir and it was uniformly dispersed in 10 minutes.
2, oil phase: the vitamin E oil of recipe quantity is preheated to 65~70 ℃.
3, emulsifying homogenizing: oil phase is slowly added water, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, gets emulsion and examines under a microscope, and answers encapsulation complete and big or small about 10 μ m, as does not reach requirement, and homogenizing is observed again.
4, spray drying: emulsion is added in the centrifugal spray dryer, and inlet temperature is 180 ℃~190 ℃, 85~90 ℃ of air-out, and the centrifugal energy nozzle rotating speed is 20,000~30,000 commentaries on classics, opens Liquid spraying pump and carries out spray drying.
5, check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
Embodiment 4
Vitamin E 65%
Arabic gum 5%
Lactose 8%
Octenyl succinate starch 20.5%
Micropowder silica gel 1.5%
Purified water is 2 times of weight of solid amount always
Preparation method:
1, water: the purified water of recipe quantity is heated to 65~70 ℃, arabic gum, octenyl succinate starch, lactose and the micropowder silica gel of recipe quantity slowly added, stir and it was uniformly dispersed in 10 minutes.
2, oil phase: the vitamin E oil of recipe quantity is preheated to 65~70 ℃.
3, emulsifying homogenizing: oil phase is slowly added water, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, gets emulsion and examines under a microscope, and answers encapsulation complete and big or small about 10 μ m, as does not reach requirement, and homogenizing is observed again.
4, spray drying: emulsion is added in the centrifugal spray dryer, and inlet temperature is 180 ℃~190 ℃, 85~90 ℃ of air-out, and the centrifugal energy nozzle rotating speed is 20,000~30,000 commentaries on classics, opens Liquid spraying pump and carries out spray drying.
Annotate: spray dryer also can be selected jet-propelled spray dryer for use.
5, check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
Embodiment 5
Vitamin E 70%
Arabic gum 2%
Dextrin 6.5%
Octenyl succinate starch 20%
Magnesium stearate 1.5%
Purified water is 2.5 times of weight of solid amount always
Preparation method:
1, water: the purified water of recipe quantity is heated to 65~70 ℃, arabic gum, octenyl succinate starch, dextrin and the magnesium stearate of recipe quantity slowly added, stir and it was uniformly dispersed in 10 minutes.
2, oil phase: the vitamin E oil of recipe quantity is preheated to 65~70 ℃.
3, emulsifying homogenizing: oil phase is slowly added water, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, gets emulsion and examines under a microscope, and answers encapsulation complete and big or small about 10 μ m, as does not reach requirement, and homogenizing is observed again.
4, spray drying: emulsion is added in the centrifugal spray dryer, and inlet temperature is 180 ℃~190 ℃, 85~90 ℃ of air-out, and the centrifugal energy nozzle rotating speed is 20,000~30,000 commentaries on classics, opens Liquid spraying pump and carries out spray drying.
Annotate: spray dryer also can be selected jet-propelled spray dryer for use.
5, check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
Embodiment 6: the chewable tablet of voltage endurance vitamin E microcapsule (microcapsule that embodiment 4 makes) preparation
Voltage endurance vitamin E microcapsule 50%
Mannitol 45%
Maltodextrin 4%
Sweeting agent is an amount of
Magnesium stearate 1%
With above-mentioned supplementary material mix homogeneously, direct compression.
Experimental result:
Outward appearance The encapsulation rate Bulk density (g/MI) Moisture Ash Content
Embodiment 1 White powder 100.0 % 4.9 2. 0% 0.4 % 49.5%
Embodiment 2 White powder 100.0 % 4.8 2. 0% 0.5 % 55.7%
Embodiment 3 White powder 98.3 % 4.8 1. 8% 0.5 % 60.2%
Embodiment 4 White powder 97.8 % 4.7 1. 8% 0.6 % 64.6%
Embodiment 5 White powder 94.3 % 4.6 1. 8% 0.6 % 70.1%
Common microcapsule Off-white powder 97.0 % 4.3 2. 5% 2.1 % 50.2%
Stability test is analyzed
The voltage endurance vitamin E microcapsule and the usual vitamin E microcapsule of embodiment 1,3,5 preparation gained are distinguished tabletting under the same conditions, be put in the accelerated test case, temperature is 40 ℃, and humidity is 75%, respectively at 1,2,3, the sampling in June, observe its outward appearance, capsule breaking rate, content; Obtain a result as following table.
1, the tablet appearance relative analysis of four kinds of different VE microcapsule preparations:
Time The tablet (outward appearance) of pressure resistant type VE microcapsule 1 preparation The tablet (outward appearance) of pressure resistant type VE microcapsule 3 preparations The tablet (outward appearance) of pressure resistant type VE microcapsule 5 preparations The tablet (outward appearance) of common VE microcapsule preparation
0 month Smooth pure white Smooth pure white Smooth pure white Smooth, unilateral have a skin dark stain
January No change No change No change Smooth, unilateral have a skin dark stain
February No change No change No change Smooth, unilateral have a skin dark stain
March No change No change No change More smooth, hardness reduces
June No change No change No change More smooth, hardness further reduces
2, the tablet microscopic examination of four kinds of different VE microcapsule preparations is (with 3.14mm 2Counting) capsule breaking rate relative analysis down:
Time The tablet (capsule breaking rate) of pressure resistant type VE microcapsule 1 preparation The tablet (capsule breaking rate) of pressure resistant type VE microcapsule 3 preparations The tablet (capsule breaking rate) of pressure resistant type VE microcapsule 5 preparations The tablet (capsule breaking rate) of common VE microcapsule preparation
0 month Broken capsule 1% Broken capsule 1% Broken capsule 5% Broken capsule 41%
January Broken capsule 2% Broken capsule 3% Broken capsule 5% Broken capsule 45%
February Broken capsule 1% Broken capsule 2% Broken capsule 6% Broken capsule 47%
March Broken capsule 1% Broken capsule 3% Broken capsule 5% Broken capsule 44%
June Broken capsule 2% Broken capsule 3% Broken capsule 6% Broken capsule 45%
3, the tablet content relative analysis of four kinds of different VE microcapsule preparations:
Time The tablet (sign content) of pressure resistant type VE microcapsule 1 preparation The tablet (sign content) of pressure resistant type VE microcapsule 3 preparations The tablet (sign content) of pressure resistant type VE microcapsule 5 preparations The tablet (sign content) of common VE microcapsule preparation
0 month 98.5% 99.5% 98.6% 97.4%
January 98.6% 99.5% 98.4% 97.0%
February 98.3% 99.3% 98.4% 96.0%
March 98.3% 99.3% 98.2% 95.5%
June 98.2% 99.0% 98.0% 93.2%
Conclusion: the tablet accelerated test of voltage endurance vitamin E microcapsule preparation was not seen significant change in 6 months, and the tablet accelerated test of usual vitamin E microcapsule preparation is after 6 months, the integrity of outward appearance, capsule and content have all produced bigger variation, illustrate that the voltage endurance vitamin E microcapsule that this experiment makes can satisfy the tabletting requirement fully.

Claims (10)

1, a kind of voltage endurance vitamin E microcapsule, it is characterized in that: the percentage by weight between its component and the component is: vitamin E oil 50%~70%, capsule material 1%~25%, auxiliary capsule material 5%~30%, octenyl succinate starch 10%~30%, fluidizer 0.5%~2%.
2, a kind of voltage endurance vitamin E microcapsule according to claim 1 is characterized in that: the capsule material is a kind of in gelatin, arabic gum, alginate, chitosan, the casein or more than 2 kinds.
3, a kind of voltage endurance vitamin E microcapsule according to claim 1 is characterized in that: auxiliary capsule material comprises a kind of in dextrin, lactose, mannitol, the sorbitol or more than 2 kinds.
4, a kind of voltage endurance vitamin E microcapsule according to claim 1 is characterized in that: fluidizer is a kind of in micropowder silica gel, Pulvis Talci, the magnesium stearate or more than 2 kinds.
5, a kind of preparation a kind of voltage endurance vitamin E microcapsule preparation method as claimed in claim 1 is characterized in that:
1), preparation aqueous phase solution: 1~3 times the purified water of always measuring admittedly by above-mentioned microcapsule component is heated to 65~70 ℃, by proportioning capsule material, octenyl succinate starch, auxiliary capsule material and fluidizer is slowly added, and stirs it to be uniformly dispersed in 8~15 minutes.
2), preparation oil phase liquid: vitamin E oil is preheated to 65~70 ℃ by proportioning.
3), the emulsifying homogenizing: above-mentioned fluid is slowly added aqueous phase solution mutually, stirring and emulsifying 30~40 minutes, homogenizing is 3 times under 40~45Mpa pressure, getting emulsion examines under a microscope, answer encapsulation complete and big or small about 10 μ m, as do not reach requirement, homogenizing is observed again;
4), spray drying: above-mentioned emulsion is added in the centrifugal spray dryer, is 180 ℃~190 ℃ in inlet temperature, 85~90 ℃ of air-out, the centrifugal energy nozzle rotating speed is under 20,000~30,000 conditions of changeing, and carries out spray drying;
5), check: finished product is carried out outward appearance, encapsulation rate, bulk density, moisture, ash, content check, qualified back packing.
6, a kind of voltage endurance vitamin E microcapsule according to claim 1, it is characterized in that: the percentage by weight between its component and the component is: vitamin E 50%, gelatin 5%, dextrin 12%, octenyl succinate starch 32%, micropowder silica gel 1%.
7, a kind of voltage endurance vitamin E microcapsule according to claim 1, it is characterized in that: the percentage by weight between its component and the component is: vitamin E 55%, sodium caseinate 9%, lactose 10%, octenyl succinate starch 25%, micropowder silica gel 1%.
8, a kind of voltage endurance vitamin E microcapsule according to claim 1, it is characterized in that: the percentage by weight between its component and the component is: vitamin E 60%, chitosan 6%, lactose 12%, octenyl succinate starch 20.8%, micropowder silica gel 1.2%.
9, a kind of voltage endurance vitamin E microcapsule according to claim 1, it is characterized in that: the percentage by weight between its component and the component is: vitamin E 65%, arabic gum 5%, lactose 8%, octenyl succinate starch 20.5%, micropowder silica gel 1.5%.
10, a kind of voltage endurance vitamin E microcapsule according to claim 1, it is characterized in that: the percentage by weight between its component and the component is: vitamin E 70%, arabic gum 2%, dextrin 6.5%, octenyl succinate starch 20%, magnesium stearate 1.5%.
CN2006100950692A 2006-08-25 2006-08-25 Voltage endurance vitamin E microcapsule and its preparing process Expired - Fee Related CN1927188B (en)

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CN102090518A (en) * 2011-01-12 2011-06-15 乐山市瑞和祥畜牧药业有限公司 Origanum oil premix and preparation method thereof
CN102716087A (en) * 2012-05-31 2012-10-10 浙江中同科技有限公司 Vitamin powder and preparation method thereof
CN101703243B (en) * 2009-08-10 2013-01-16 北京市金康普食品添加剂科技有限公司 Vitamin e powder and preparation method thereof
CN105542234A (en) * 2016-01-25 2016-05-04 中国农业科学院农产品加工研究所 Degradable composite film for cold fresh meat
CN106262933A (en) * 2016-11-08 2017-01-04 浙江工业大学 A kind of preparation method of Vitamin E contained micro capsule
CN108888601A (en) * 2018-08-02 2018-11-27 济源希健生物医药科技发展有限公司 A kind of vitamin E selenium microcapsules tablet, preparation method and its usage
CN109619536A (en) * 2018-10-18 2019-04-16 山东海能生物工程有限公司 A kind of 25-hydroxy-vitamin D3Microcapsule powder and preparation method thereof
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

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US6020003A (en) * 1998-02-23 2000-02-01 Basf Corporation Method of making spray-dried powders with high edible-oil loadings based on non-hydrolyzed gelatin
EP0966889B1 (en) * 1998-06-24 2007-05-02 DSM IP Assets B.V. Vitamin powders for beverage applications
EP1066761B1 (en) * 1999-07-06 2004-09-29 DSM IP Assets B.V. Compositions containing fat-soluble substances in a carbohydrate matrix
CN1203843C (en) * 2001-04-10 2005-06-01 中国科学院成都有机化学研究所 Preparation method of high-content oil-soluble vitamin slow-releasing microcapsule powder

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CN101703243B (en) * 2009-08-10 2013-01-16 北京市金康普食品添加剂科技有限公司 Vitamin e powder and preparation method thereof
CN102090518A (en) * 2011-01-12 2011-06-15 乐山市瑞和祥畜牧药业有限公司 Origanum oil premix and preparation method thereof
CN102716087A (en) * 2012-05-31 2012-10-10 浙江中同科技有限公司 Vitamin powder and preparation method thereof
CN102716087B (en) * 2012-05-31 2014-06-11 浙江中同科技有限公司 Vitamin powder and preparation method thereof
CN105542234A (en) * 2016-01-25 2016-05-04 中国农业科学院农产品加工研究所 Degradable composite film for cold fresh meat
CN105542234B (en) * 2016-01-25 2018-02-13 中国农业科学院农产品加工研究所 Degradable composite membrane for cold fresh meat
CN106262933A (en) * 2016-11-08 2017-01-04 浙江工业大学 A kind of preparation method of Vitamin E contained micro capsule
CN108888601A (en) * 2018-08-02 2018-11-27 济源希健生物医药科技发展有限公司 A kind of vitamin E selenium microcapsules tablet, preparation method and its usage
CN109619536A (en) * 2018-10-18 2019-04-16 山东海能生物工程有限公司 A kind of 25-hydroxy-vitamin D3Microcapsule powder and preparation method thereof
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

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