CN100558345C - The preparation method of the nano-sphere/microsphere double-embedding system of a kind of vitamin A, vitamin E - Google Patents

Abstract

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.The present invention is the nanosphere core with the food stage vitamin A, monoglyceride or Cera Flava are nanosphere wall material, make the nanosphere suspension, with vitamin E as the microsphere core, the octenyl succinate starch that contains tween 80 adopts thermally homogenising-spray drying method for preparation nano-sphere/microsphere double-embedding system as microsphere wall material.The vitamin A nanosphere that the present invention makes can reach 82%～94% to the envelop rate of vitamin A, and the nanosphere particle diameter is 200nm～370nm.Double-embedding system reaches 86%～91% to the envelop rate of vitamin A, and the envelop rate of vitamin E reaches 89%～93%; This double-embedding system is embedding vitamin A, E simultaneously, and the effect that has substep to discharge, and to avoid the mutual interference of active component phase, improves bioavailability, can be used as the vitamin reinforcing agent, supplement add in the numerous food.

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, the mass ratio of tween 80 and octenyl succinate starch is 1: 40-50, and the mass ratio of octenyl succinate starch and monoglyceride or peak wax is 5-8: 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 kind of 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, the mass ratio of tween 80 and octenyl succinate starch is 1: 40-50, and the mass ratio of octenyl succinate starch and monoglyceride or peak wax is 5-8: 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.

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