CN101214219A - Method for preparing vitamin A and vitamin E nano-sphere/microsphere double-embedding system - Google Patents

Method for preparing vitamin A and vitamin E nano-sphere/microsphere double-embedding system Download PDF

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Publication number
CN101214219A
CN101214219A CNA2007101920237A CN200710192023A CN101214219A CN 101214219 A CN101214219 A CN 101214219A CN A2007101920237 A CNA2007101920237 A CN A2007101920237A CN 200710192023 A CN200710192023 A CN 200710192023A CN 101214219 A CN101214219 A CN 101214219A
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vitamin
embedding
nano
sphere
double
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CN100558345C (en
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许时婴
夏书芹
许婧
朱卫红
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Jiangnan University
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Jiangnan University
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Abstract

A preparation method of vitamin A and vitamin E nano-sphere/microsphere double-embedding system belongs to the technical field of biological active substance control release microencapsulation. In the present invention, food grade vitamin A is nano-sphere core material and monoglyceride or beeswax is nano-sphere wall material to be made into nano-sphere suspension which is used as microsphere core material together with the vitamin E; ocentyl succinate esterified starch containing tween-80 is used as microsphere wall material; the nano-sphere/microsphere double-embedding system is manufactured by a thermal homogenization-spray drying method. The encapsulation rate towards the vitamin A of vitamin A nano-sphere manufactured by the present invention can reach to 82 percent to 94 percent, and the particle size of the nano-sphere is 200nm to 370nm. The encapsulation rate towards the vitamin A of the double-embedding system is 86 percent to 91 percent and the encapsulation rate towards the vitamin E is 89 percent to 93 percent. The double-embedding system can embed the vitamin A and the vitamin E synchronously and has the effect of releasing step be step, so as to avoid the mutual interference of active components, improve the biological utilization rate and can be added into various foods as vitamin intensifier and extender.

Description

The preparation method of the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E
Technical field
The preparation method of the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E belongs to the microencapsulation technology field of bioactive substance sustained release.
Background technology
Vitamin A is that the human body normal growth is grown, skeleton forms, keeps normal vision and immune essential nutrient element, has anti peroxidation of lipid, and enhance immunity strengthens infection, regulates the fat storage, improves functions such as iron deficiency anemia.(vitamin A deficiency VAD) is the community nutrition problem that many developing countries exist to the shortage of vitamin A.Vitamin A deficiency has improved various infectious disease, respiratory tract disease and diarrheal M ﹠ M.
Vitamin E is the fat-soluble Natural antioxidant, suppresses lipid peroxidation by the active of passivation peroxylradicals or with the lipid peroxidation radical reaction, helps to improve immunity and disease preventing and treating, influences gene transcription and expression.Vitamin E also has defying age, human body immunity improving power, the disorderly various diseases that causes of prevention Radical Metabolism and prevention presenile senile dementia, antitumor, prevents the effect of the aspects such as radiation damage of DNA, is the focus that people study always.At present, start one natural Vitamin E heat abroad, consume 2500~3000 tons every year, and, become the supplement of widely used disease-prevention health, life lengthening in American-European countries's mid-aged population with annual 10% speed increment.But the easy oxidation of vitamin, tool heliosensitivity, thermal sensitivity, so the embedding techniques of vitamin A, vitamin E also becomes the focus of research.
Studies show that vitamin A excessive adds the absorption that can disturb vitamin E, causes the generation of vitamin e deficiency when serious.High-caliber vitamin A is partly degraded at intestinal and is produced retinol and tretinoin, promotes that alpha-tocopherol is oxidized to the fertility quinone, and promotes alpha-tocopherol to discharge from blood plasma by the generation that improves gluconic acid in vivo.Therefore, for the multiple bioactive substance of while embedding, interfering with each other when preventing its metabolism also is very important aspect, therefore just needs the multilamellar embedding, provides substep to discharge.
For single fatsoluble vitamin, the domestic hydrophilic wall material of mostly selecting carries out embedding, but this class wall material can not provide effective slow releasing function, and is promptly dissolved after the wall material is met water (as saliva), thereby causes a large amount of releases of core.Wang Hua etc. prepare type vitamin A microcapsules with complex coacervation, but complex coacervation last handling process difficulty is big, are difficult for preserving, even after the spray drying, capsule particle is rounding no longer, but flocks together.Up to now, the domestic report of not seeing relevant for the double-layer embedment of vitamin A, vitamin E.
Summary of the invention
The preparation method that the purpose of this invention is to provide the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E controlled release, for the method for various active material embedding simultaneously is provided, avoid phase mutual interference between the active substance, to reach the effect of slow release and controlled release, improve the bioavailability of vitamin A, E.
Technical scheme of the present invention: the preparation method of the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E, this system layering embedding vitamin A, vitamin E, and substep discharges vitamin A, vitamin E; Preparation process is:
(1) preparation is the nanosphere suspension of wall material embedding vitamin A with monoglyceride or peak wax: under 70 ℃ with the fusion of wall material, adding vitamin A makes it to mix, the carrying capacity of vitamin A is 20% in mass in mixture, and promptly 1 part of vitamin A oil is equipped with 4 parts of monoglycerides or peak wax; Be distributed to then in the octenyl succinate starch solution that has added tween 80, tween 80 is 1 with the quality ratio of octenyl succinate starch: 40-50, and octenyl succinate starch is 5-8 with the quality ratio of monoglyceride or peak wax: 1; 10000r/min high speed dispersion 30s in 70~80 ℃ of high pressure homogenize under 40~60MPa, repeats 3 times, cools off fast in ice-water bath, gets the nanosphere suspension of embedding vitamin A;
(2) the nano-sphere/microsphere double-embedding suspension of preparation vitamin A, vitamin E: in the nanosphere suspension of the embedding vitamin A that step (1) makes, add vitamin E while stirring, solid content is 38%~42% in mass; 20500r/min high speed dispersion 1min in 70~80 ℃ of high pressure homogenize under 40~60MPa, repeats 3 times, cools off fast in ice-water bath, gets the nano-sphere/microsphere double-embedding suspension of embedding vitamin A, vitamin E;
(3) spray drying prepares double-embedding system: it is 38%~42% in mass that the suspension solid content is buried in the double-contracting for preparing, 185~190 ℃ of inlet temperature, and 80~90 ℃ of leaving air temps, spray drying makes double-embedding system.
The mensuration of nanosphere particle diameter: adopt the dynamic light scattering particle size instrument to measure, measure 25 ℃ of temperature.The envelop rate of vitamin A and vitamin E adopts high-performance liquid chromatogram determination.
Vitamin A nanosphere mean diameter is 200nm~370nm, and double-embedding system can reach 86~91% to the envelop rate of vitamin A, and the envelop rate of vitamin E can reach 89~93%.
Beneficial effect of the present invention: with the food stage vitamin A is the nanosphere core, monoglyceride or Cera Flava are nanosphere wall material, make the nanosphere suspension, with vitamin E as the microsphere core, the octenyl succinate starch that has added tween 80 adopts thermally homogenising-spray drying method for preparation nano-sphere/microsphere double-embedding system as microsphere wall material.The method of multiple bioactive substance embedding simultaneously is provided, avoids phase mutual interference between the bioactive substance, and reach the effect of slow release and controlled release, to improve the bioavailability of bioactive substance.
Description of drawings
Fig. 1 nanosphere particle size distribution figure.
Fig. 2 nano-sphere/microsphere double-embedding system stereoscan photograph.
The specific embodiment
Embodiment 1
Accurately take by weighing monoglyceride 20g, under 70 ℃, heating makes it fusion, accurately takes by weighing vitamin A oil 5g, joins in the fused monoglyceride stirring and evenly mixing.Accurately take by weighing 160g and added the octenyl succinate starch (modified starch Hi-CAP100) of tween 80, under 70 ℃, be dissolved in the 600mL water, the fusion monoglyceride that has added vitamin A is added in the modified starch Hi-CAP100 solution, the powerful stirring, high speed dispersion (10000r/min, 30s).Accurately take by weighing vitamin E oil 55g, add in the above-mentioned modified starch solution, and high speed dispersion (20500r/min, 1min), high pressure homogenize (40MPa) repeats 3 times, and all operations all carries out under 70 ℃.In ice-water bath, be cooled to rapidly below the monoglyceride fusing point, spray drying, 190 ℃ of inlet temperature, 90 ℃ of leaving air temps, the nano-sphere/microsphere double-embedding system of embedding vitamin A, vitamin E.
Embodiment 2
Accurately take by weighing monoglyceride 42g, under 70 ℃, heating makes it fusion, accurately takes by weighing vitamin A oil 10.5g, joins in the fused monoglyceride stirring and evenly mixing.Accurately take by weighing 340g modified starch Hi-CAP100, under 70 ℃, be dissolved in the 1050mL water, the fusion monoglyceride that has added vitamin A is added in the modified starch Hi-CAP100 solution, the powerful stirring, high speed dispersion (10000r/min, 30s).Accurately take by weighing vitamin E oil 52g, add in the above-mentioned modified starch solution, and high speed dispersion (20500r/min, 1min), high pressure homogenize (60MPa) repeats 3 times, and all operations all carries out under 70 ℃.In ice-water bath, be cooled to rapidly below the monoglyceride fusing point, spray drying, 190 ℃ of inlet temperature, 90 ℃ of leaving air temps promptly get the nano-sphere/microsphere double-embedding system of embedding vitamin A, vitamin E.
Embodiment 3
Accurately take by weighing Cera Flava 30g, under 78 ℃, heating makes it fusion.Accurately take by weighing vitamin A 7.5g, join in the fused Cera Flava stirring and evenly mixing.Accurately take by weighing 150g modified starch Hi-CAP100, under 78 ℃, be dissolved in the 570mL water, the fusion Cera Flava that has added vitamin A is joined in the modified starch Hi-CAP100 solution, the powerful stirring, high speed dispersion (10000r/min, 30s).Accurately take by weighing vitamin E 39g, add in the above-mentioned modified starch solution, and high speed dispersion (20500r/min, 1min), high pressure homogenize (50MPa) repeats 3 times, and all operations all carries out under 78 ℃.In ice-water bath, be cooled to rapidly below the Cera Flava fusing point, spray drying, 185 ℃ of inlet temperature, 85 ℃ of leaving air temps promptly get the nano-sphere/microsphere double-embedding system of embedding vitamin A, vitamin E.

Claims (1)

1. the preparation method of the nano-sphere/microsphere double-embedding system of a vitamin A, vitamin E is characterized in that this system layering embedding vitamin A, vitamin E, and substep discharges vitamin A, vitamin E; Preparation process is:
(1) preparation is the nanosphere suspension of wall material embedding vitamin A with monoglyceride or peak wax: under 70 ℃ with the fusion of wall material, adding vitamin A makes it to mix, the carrying capacity of vitamin A is 20% in mass in mixture, and promptly 1 part of vitamin A is equipped with 4 parts of monoglycerides or peak wax; Be distributed to then in the octenyl succinate starch solution that has added tween 80, tween 80 is 1 with the quality ratio of octenyl succinate starch: 40-50, and octenyl succinate starch is 5-8 with the quality ratio of monoglyceride or peak wax: 1; 10000r/min high speed dispersion 30s in 70~80 ℃ of high pressure homogenize under 40~60MPa, repeats 3 times, cools off fast in ice-water bath, gets the nanosphere suspension of embedding vitamin A;
(2) the nano-sphere/microsphere double-embedding suspension of preparation vitamin A, vitamin E: in the nanosphere suspension of the embedding vitamin A that step (1) makes, add vitamin E while stirring, solid content is 38%~42% in mass; 20500r/min high speed dispersion 1min in 70~80 ℃ of high pressure homogenize under 40~60MPa, repeats 3 times, cools off fast in ice-water bath, gets the nano-sphere/microsphere double-embedding suspension of embedding vitamin A, vitamin E;
(3) spray drying prepares double-embedding system: it is 38%~42% in mass that the suspension solid content is buried in the double-contracting for preparing, 185~190 ℃ of inlet temperature, and 80~90 ℃ of leaving air temps, spray drying makes double-embedding system.
CNB2007101920237A 2007-12-28 2007-12-28 The preparation method of the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E Expired - Fee Related CN100558345C (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
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CN102198116A (en) * 2011-05-30 2011-09-28 何德海 Preparation method of vitamin A microcapsules
CN102362864A (en) * 2011-10-26 2012-02-29 浙江新维普添加剂有限公司 Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules
CN101502326B (en) * 2009-02-23 2012-06-27 江南大学 Method for preparing vitamin E nano liposome
CN104351473A (en) * 2014-10-22 2015-02-18 浙江万方生物科技有限公司 Preparation method of water-soluble multivitamin micropills for livestock and poultry
CN104473168A (en) * 2014-12-26 2015-04-01 江南大学 Processing method for increasing solubility and bioavailability of fat-soluble active component
US9173818B2 (en) 2011-03-25 2015-11-03 Zhejiang Nhu Company Ltd Method for preparing stable-type vitamin A microcapsules continuously
CN110820358A (en) * 2019-10-25 2020-02-21 嘉兴市秀洲恒丰纺织有限公司 Finishing process of vitamin skin-care health-care real silk fabric
CN111803405A (en) * 2020-08-10 2020-10-23 江南大学 Microcapsule for essence and medicine amorphous and preparation method thereof
WO2020221052A1 (en) * 2019-04-28 2020-11-05 中国科学院上海药物研究所 Alpha-tocopherol microsphere and preparation method therefor
CN111992153A (en) * 2020-08-10 2020-11-27 江南大学 High-loading-capacity high-thermal-stability menthol microcapsule and preparation method thereof
CN113016864A (en) * 2021-04-20 2021-06-25 甘肃农业大学 Preparation method of dried meat preservative
CN115381104A (en) * 2022-08-10 2022-11-25 新昌新和成维生素有限公司 Preparation method and device of vitamin A microcapsules

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101502326B (en) * 2009-02-23 2012-06-27 江南大学 Method for preparing vitamin E nano liposome
US9173818B2 (en) 2011-03-25 2015-11-03 Zhejiang Nhu Company Ltd Method for preparing stable-type vitamin A microcapsules continuously
CN102198116A (en) * 2011-05-30 2011-09-28 何德海 Preparation method of vitamin A microcapsules
CN102362864A (en) * 2011-10-26 2012-02-29 浙江新维普添加剂有限公司 Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules
CN102362864B (en) * 2011-10-26 2013-03-13 浙江新维普添加剂有限公司 Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules
CN104351473A (en) * 2014-10-22 2015-02-18 浙江万方生物科技有限公司 Preparation method of water-soluble multivitamin micropills for livestock and poultry
CN104351473B (en) * 2014-10-22 2018-02-02 刘希悦 A kind of preparation method of Aquavite micropill for livestock and poultry
CN104473168A (en) * 2014-12-26 2015-04-01 江南大学 Processing method for increasing solubility and bioavailability of fat-soluble active component
WO2020221052A1 (en) * 2019-04-28 2020-11-05 中国科学院上海药物研究所 Alpha-tocopherol microsphere and preparation method therefor
CN110820358A (en) * 2019-10-25 2020-02-21 嘉兴市秀洲恒丰纺织有限公司 Finishing process of vitamin skin-care health-care real silk fabric
CN111803405A (en) * 2020-08-10 2020-10-23 江南大学 Microcapsule for essence and medicine amorphous and preparation method thereof
CN111992153A (en) * 2020-08-10 2020-11-27 江南大学 High-loading-capacity high-thermal-stability menthol microcapsule and preparation method thereof
CN111992153B (en) * 2020-08-10 2022-10-18 江南大学 High-loading-capacity high-thermal-stability menthol microcapsule and preparation method thereof
CN111803405B (en) * 2020-08-10 2023-08-22 江南大学 Microcapsule capable of being used for essence and preparation method thereof
CN113016864A (en) * 2021-04-20 2021-06-25 甘肃农业大学 Preparation method of dried meat preservative
CN113016864B (en) * 2021-04-20 2023-11-28 甘肃农业大学 Preparation method of jerky preservative
CN115381104A (en) * 2022-08-10 2022-11-25 新昌新和成维生素有限公司 Preparation method and device of vitamin A microcapsules
CN115381104B (en) * 2022-08-10 2024-04-02 新昌新和成维生素有限公司 Preparation method and device of vitamin A microcapsule

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