CN102198116A - Preparation method of vitamin A microcapsules - Google Patents
Preparation method of vitamin A microcapsules Download PDFInfo
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- CN102198116A CN102198116A CN 201110142578 CN201110142578A CN102198116A CN 102198116 A CN102198116 A CN 102198116A CN 201110142578 CN201110142578 CN 201110142578 CN 201110142578 A CN201110142578 A CN 201110142578A CN 102198116 A CN102198116 A CN 102198116A
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Abstract
The invention relates to a preparation method of more stable vitamin A microcapsules, comprising the following steps of: firstly, preparing a vitamin A oil solution containing an antioxidant from vitamin A and the antioxidant in the absence of oxygen, adding chitosan and stirring evenly, after stirring fully, filtering and removing the chitosan to obtain the vitamin A oil solution; adding octenyl succinic acid modified starch to purified water deaerated by a thermal spray deaerator, heating for dissolution; mixing the prepared octenyl succinic acid modified starch solution and the vitamin A oil solution in a certain proportion, emulsifying quickly by an on-line emulsifying machine, and instantly cooling by a cooler; and performing hot air spray drying on the emulsion to obtain stable vitamin A microcapsules. The storage life of the product prepared in the invention reaches two years.
Description
Technical field
The present invention relates to a kind of preparation technology of stable type vitamin A microcapsules, relate to the employing quick emulsification, the preparation method of the instantaneously cooled type vitamin A microcapsules of emulsion.
Background technology
Vitamin A is to keep the necessary a kind of material of people's bulk-growth, growth, reproduction and cell membrane stability.Vitamin A is to low light level sensitivity, and is relevant with scotopic vision, can cause nyctalopia during shortage; It can keep the complete of epithelial tissue structure with sound, causes dry hypertrophy of epithelium and keratinization during shortage, easily causes infection, to eye, and respiratory tract, digestive tract, the influence of urinary tract and reproductive system epithelium is remarkable; The long-term lacking vitamin A, the tear glandular epithelium is unsound, and tear reduce, and can develop into xerophthalmia and keratomalacia, and companion's perforation of cornea is blind at last; Vitamin A also can promote growth normal, and bone growth is bad during shortage, and growth promoter is obstructed, the reproductive function decline.The child needs vitamin A 0.45-1.5mg every day, and the adult then is 1.5-3mg.
Vitamin A is a fatsoluble vitamin, is soluble in organic solvent and fat, and chance heat, light, soda acid, oxygen and heavy metal etc. are all perishable, and generally being processed into microcapsule could use.Microcapsule technology is with solid, and the liquids and gases material is embedded in the microencapsulation, becomes a kind of technology of solid particle.This technology can make by the material of embedding and external environment isolates, reduce effectively by diffusion and the evaporation of embedding substance to environment, cover by the abnormal flavour of the material of embedding, keep its original color, smell and taste to greatest extent, physicochemical property and biological activity, prevent that nutritional labeling is destroyed, and have the function of slow release.The preparation type vitamin A microcapsules generally with vitamin A oil with emulsifying agent emulsifying, with emulsion spray drying or mist projection granulating, obtain through fluidized drying again.
Chinese patent CN1965657 (A) has introduced a kind of preparation method of flour nutrition intensifying Vitamin A microcapsule, this method is the wall material with ocentyl succinic powder ester HI-CAP100, with the vitamin A oil was core, at 5000-20000 rev/min of following high speed dispersion 1-2 minute.And then homogenizing 2 times under the 10-40Mpa, then spray-dried preparation microcapsule, the microcapsule mean diameter of preparation is 85.6 microns.And Chinese patent CN101214219 (A) has introduced the preparation vitamin A, and the method for Vitamin E contained micro capsule has been used the high shear under the 10000-20500rpm rotating speed in its emulsion process, and homogenizing is 3 times under 40-60Mpa, and then spray drying prepares microcapsule.The aforesaid way preparation easily causes vitamin A rotten because the emulsifying temperature height is operated in open environment again; Simultaneously because emulsion system instability, the easy layering of emulsion in spray-drying process after emulsifying is finished, accumulative oil droplet easily forms bulky grain, thereby influences the embedding effect and the bioavailability of final products.
Chinese patent CN101513394 (A) has reported the preparation method of serialization nanometer dispersed vitamin A microcapsule.Vitamin A crystal is ground to vitamin A particle diameter 2-5 micron with the antioxidant solvent; be made into the vitamin A dispersion liquid; after the rising temperature for dissolving; cooling enters in the hypergravity RPB crystallize device of liquid distribution trough; the aqueous solution that will contain protecting colloid simultaneously is with being pumped in this hypergravity RPB crystallize device; obtain the vitamin A dispersion liquid of nano-dispersed, spray drying obtains type vitamin A microcapsules.Owing to adopt above-mentioned continuous nano-dispersed to prepare type vitamin A microcapsules then in using dissolving agent process, can bring the dissolvent residual in the product, can't obtain the product of better quality.
Chinese patent CN101744790 (A) has introduced a kind of preparation method of stable-type vitamin A microcapsules continuously; under nitrogen protection; vitamin A crystal and antioxidant are made into the molten oil of the vitamin A that contains antioxidant; with being pumped in the hypergravity RPB emulsator that has liquid distribution trough; but the aqueous solution that will contain gelation modification powder simultaneously after deoxidation treatment with being pumped into above-mentioned hypergravity RPB emulsator; obtain the vitamin A emulsion, spray drying obtains type vitamin A microcapsules.Adopt above-mentioned hypergravity RPB emulsator, then its emulsifying power is not as high-shear emulsion machine; In addition, used water will damage vitamin A in the preparation process if do not carry out deoxidation treatment in the emulsifying.
The inventor has proposed a kind of better technical matters to obtain the final products of better quality at the problems referred to above.
Summary of the invention
The present invention is directed to the disappearance of prior art existence, its main purpose provides a kind of preparation method of more stable type vitamin A microcapsules.
For achieving the above object, the present invention adopts as the purgation technical scheme: a kind of preparation method of more stable type vitamin A microcapsules, and it may further comprise the steps:
One, under anaerobic state, vitamin A and antioxidant are pressed 100:(0.05～0.5) weight ratio even in (50～65) ℃ following stirring and dissolving, be made into the vitamin A oil solution that contains antioxidant; Adding the vitamin A oil percentage by weight under this temperature is the chitosan of (0.1～0.5) %, stirs 45 minutes;
Two, the vitamin A oil solution that is added with chitosan filters by filter press, and the elimination chitosan is fully removed the vitamin A oil solution of heavy metal;
Three, purified water is passed through the abundant deoxygenation of thermal spraying oxygen eliminator, drop into then in the dissolving pan of anaerobic state; Then new starch alkenyl succinate ester input has been added in the emulsifying pot of anaerobic water, heating for dissolving, solution temperature are (50～65) ℃, and mixing time 20 minutes is to be made into the new starch alkenyl succinate ester solution of (40～50) %;
Four, will remove vitamin A oil solution after the heavy metal and new starch alkenyl succinate ester solution sends into online mulser and carries out quick emulsification, emulsion is cooled to (20～30) ℃ by cooler, enter in the pans of anaerobic state, vitamin A oil is 1:(2～4 with the weight ratio of new starch alkenyl succinate ester in the vitamin A emulsion that obtains);
Five, said vitamin A emulsion is carried out hot-air spray drying, wherein adjust inlet temperature and be (200～240) ℃, leaving air temp (90～130) ℃ finally obtains type vitamin A microcapsules through hot-air spray drying.
Described antioxidant is a natural VE, and natural VE contains 50% tocopherol; The anaerobic state of described preparation process is meant in the container fills up protective gas behind the evacuation, as nitrogen, carbon dioxide, argon, is preferably nitrogen.
After the present invention adopted technique scheme, its beneficial effect was: vitamin A is a kind of fatsoluble vitamin of poor stability, is having under light, oxygen, heavy metal, oxidant, soda acid existence and the higher temperature environment, and its effective content can obviously descend.The present invention adopts chitosan that vitamin A oil is carried out the removal of residual heavy metal, makes vitamin A avoid the influence of heavy metal, and the microcapsule of making is more stable.Chitosan is a kind of nontoxic material, and the amino and the carboxyl of its molecule play chelatingligand, is high performance heavy metal chelating agent therefore.Removing the response rate and can reach (95-100) % for metal ion.Vitamin A oil fails to detect the heavy metal in the oil through the absorption of chitosan.The microcapsule preparation process is all carried out in anaerobic state, and used purified water is through deoxidation treatment, and preparation process can not damage vitamin A, improves outer field resistance oxygen of type vitamin A microcapsules and oxidation resistance.The emulsifying of vitamin A oil uses the online-emulsification machine to carry out quick emulsification, has avoided the destruction that the emulsion process temperature is higher, the time causes vitamin A than length.The timely cooling of emulsion makes vitamin A avoid Temperature Influence, and the micro encapsulation process obtains better protection.Core of the present invention is that production process carried out going heavy metal to handle to vitamin A oil; operate under the anaerobic state and carry out, short emulsification times, lower emulsion temperature; effectively the protection vitamin A is not subjected to the influence of external environment factor, guarantees the stability of type vitamin A microcapsules product.
The specific embodiment:
The present invention is described in detail below in conjunction with specific embodiment:
Embodiment 1:
In advance oleo kettle is carried out anaerobic state operation, i.e. evacuation, vacuum reaches-more than the 0.9Mpa, close vacuum valve, replenish nitrogen to normal pressure.Open charge door after the repetitive operation three times, crack nitrogen adds vitamin A 50KG, natural VE oil 25g.Close charge door, fill a vacuum at evacuation with nitrogen.Open and stir, temperature is 55 ℃ in being heated to.Crack nitrogen is opened charge door, adds chitosan 0.05kg, stirs 45 minutes.Filter by dish formula filter while hot, obtain vitamin A oil solution.
The purified water of 250kg by the thermal spraying deoxygenation, is added in the dissolving pan of deoxygenation, and then dropping into model is the national starch 100kg of HI-CAP100,, be made into 40% new thiazolinyl succinum starch ester solution.Dissolving pan is again after the deoxygenation, heating for dissolving.50～60 ℃ of solution temperatures stirred 20 minutes.
Vitamin A oil that dissolving is good and new thiazolinyl succinum starch ester solution enter the online-emulsification machine in the ratio of 1:2, and the material after the emulsifying is cooled to 20 ℃ by cooler, enters in the pans of anaerobic state, carries out spray drying immediately.200～240 ℃ of spray drying inlet temperature, 90～130 ℃ of leaving air temps obtain type vitamin A microcapsules.Microcapsule embedded rate is 99.6%, detects through HPLC, and the content of vitamin A is 51.6 million international units.Normal temperature storage 2 years, content are 50.3 million international units, and content descends 2.5%.
Embodiment 2:
In advance oleo kettle is carried out anaerobic state operation, i.e. evacuation, vacuum reaches-more than the 0.9Mpa, close vacuum valve, replenish nitrogen to normal pressure.Open charge door after the repetitive operation three times, crack nitrogen adds vitamin A 50KG, natural VE oil 50g.Close charge door, again evacuation and fill a vacuum with nitrogen.Open and stir, temperature is 55 ℃ in being heated to.Crack nitrogen is opened charge door, adds chitosan 0.025kg, stirs 45 minutes.Filter by dish formula filter while hot, obtain vitamin A oil solution.
The purified water of 330kg by the thermal spraying deoxygenation, is added in the dissolving pan of deoxygenation, and then dropping into model is the national starch 150kg of HI-CAP100,, be made into 45% new thiazolinyl succinum starch ester solution.Dissolving pan is again after the deoxygenation, heating for dissolving.50～60 ℃ of solution temperatures stirred 20 minutes.
Vitamin A oil that dissolving is good and new thiazolinyl succinum starch ester solution enter the online-emulsification machine in the ratio of 1:2, and the material after the emulsifying is cooled to 25 ℃ by cooler, enters in the pans of anaerobic state, carries out spray drying immediately.200～240 ℃ of spray drying inlet temperature, 90～130 ℃ of leaving air temps obtain type vitamin A microcapsules.Microcapsule embedded rate is 99.7%, detects through HPLC, and the content of vitamin A is 38.9 million international units.Normal temperature storage 2 years, content are 37.1 million international units, and content descends 2.7%.
Embodiment 3:
In advance oleo kettle is carried out anaerobic state operation, i.e. evacuation, vacuum reaches-more than the 0.9Mpa, close vacuum valve, replenish nitrogen to normal pressure.Open charge door after the repetitive operation three times, crack nitrogen adds vitamin A 50KG, and tocopherol content is 50% natural VE oil 250g.Close charge door, fill a vacuum at evacuation with nitrogen.Open and stir, temperature is 55 ℃ in being heated to.Crack nitrogen is opened charge door, adds chitosan 0.25kg, stirs 45 minutes.Filter by dish formula filter while hot, obtain vitamin A oil solution.
The purified water of 400kg by the thermal spraying deoxygenation, is added in the dissolving pan of deoxygenation, and then dropping into model is the national starch 200kg of HI-CAP100,, be made into 50% new thiazolinyl succinum starch ester solution.Dissolving pan is again after the deoxygenation, heating for dissolving.50～60 ℃ of solution temperatures stirred 20 minutes.
Vitamin A oil that dissolving is good and new thiazolinyl succinum starch ester solution enter the online-emulsification machine in the ratio of 1:2, and the material after the emulsifying is cooled to 30 ℃ by cooler, enters in the pans of anaerobic state, carries out spray drying immediately.200～240 ℃ of spray drying inlet temperature, 90～130 ℃ of leaving air temps obtain type vitamin A microcapsules.Microcapsule embedded rate is 99.4%, detects through HPLC, and the content of vitamin A is 31.2 million international units.Normal temperature storage 2 years, content are 30.3 million international units, and content descends 2.9%.
Of the present invention focusing on adopts chitosan that vitamin A oil is carried out the removal of residual heavy metal, makes vitamin A avoid the influence of heavy metal, and the microcapsule of making is more stable.Chitosan is a kind of nontoxic material, and the amino and the carboxyl of its molecule play chelatingligand, is high performance heavy metal chelating agent therefore.Removing the response rate and can reach (95-100) % for metal ion.Vitamin A oil fails to detect the heavy metal in the oil through the absorption of chitosan.The microcapsule preparation process is all carried out in anaerobic state, improves the outer field resistance oxygen of type vitamin A microcapsules.Used purified water is through deoxidation treatment, and preparation process can not damage vitamin A, improves outer field resistance oxygen of type vitamin A microcapsules and oxidation resistance.The emulsifying of vitamin A oil uses the online-emulsification machine to carry out quick emulsification, has avoided the destruction that the emulsion process temperature is higher, the time causes vitamin A than length.The timely cooling of emulsion makes vitamin A avoid Temperature Influence, and the micro encapsulation process obtains better protection.Core of the present invention is that production process carried out going heavy metal to handle to vitamin A oil; operate under the anaerobic state and carry out, short emulsification times, lower emulsion temperature; effectively the protection vitamin A is not subjected to the influence of external environment factor, guarantees the stability of type vitamin A microcapsules product.
The above, it only is preferred embodiment of the present invention, be not that technical scope of the present invention is imposed any restrictions, so every foundation technical spirit of the present invention all still belongs in the scope of technical solution of the present invention any trickle modification, equivalent variations and modification that above embodiment did.
Claims (6)
1. the preparation method of a type vitamin A microcapsules, it is characterized in that: this preparation method may further comprise the steps:
One, under anaerobic state, vitamin A and antioxidant are pressed 100:(0.05～0.5) weight ratio even in (50～65) ℃ following stirring and dissolving, be made into the vitamin A oil solution that contains antioxidant; Adding the vitamin A oil percentage by weight under this temperature is the chitosan of (0.1～0.5) %, stirs 45 minutes;
Two, the above-mentioned vitamin A oil solution that is added with chitosan is filtered by filter press, the elimination chitosan is fully removed the vitamin A oil solution of heavy metal;
Three, purified water is passed through the abundant deoxygenation of thermal spraying oxygen eliminator, drop into then in the dissolving pan of anaerobic state; Then new starch alkenyl succinate ester input has been added in the emulsifying pot of anaerobic water, heating for dissolving, solution temperature are (50～65) ℃, and mixing time 20 minutes is to be made into the new starch alkenyl succinate ester solution of (40～50) %;
Four, will remove vitamin A oil solution after the heavy metal and new starch alkenyl succinate ester solution sends into online mulser and carries out quick emulsification, emulsion is cooled to (20～30) ℃ by cooler, enter in the pans of anaerobic state, vitamin A oil is 1:(2～4 with the weight ratio of new starch alkenyl succinate ester in the vitamin A emulsion that obtains);
Five, said vitamin A emulsion is carried out hot-air spray drying, wherein adjust inlet temperature and be (200～240) ℃, leaving air temp (90～130) ℃ finally obtains type vitamin A microcapsules through hot-air spray drying.
2. the preparation method of the type vitamin A microcapsules of telling according to claim 1, it is characterized in that: described antioxidant is a natural VE.
3. the preparation method of the type vitamin A microcapsules of telling according to claim 2, it is characterized in that: described natural VE contains 50% tocopherol.
4. according to the preparation method of the type vitamin A microcapsules of telling according to claim 1, it is characterized in that: national of the United States's starch that described new starch alkenyl succinate ester is model HI-CAP100.
5. according to the preparation method of each described type vitamin A microcapsules of claim 1 to 4, it is characterized in that: described anaerobic state is meant in the container fills up protective gas behind the evacuation.
6. the preparation method of type vitamin A microcapsules according to claim 5, it is characterized in that: described protective gas is nitrogen, carbon dioxide or argon.
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Cited By (6)
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| CN103976353A (en) * | 2014-04-24 | 2014-08-13 | 武汉星辰现代生物工程有限公司 | Beta-carotene microcapsule production method |
| CN104522681A (en) * | 2015-01-10 | 2015-04-22 | 黄家亨 | Vitamin A absorption promoter and corresponding vitamin A replenisher comprising same |
| CN105456235A (en) * | 2015-11-20 | 2016-04-06 | 厦门金达威维生素有限公司 | High-stability and high-potency-unit vitamin A oil and preparation method thereof |
| CN106579407A (en) * | 2016-12-02 | 2017-04-26 | 南通励成生物工程有限公司 | Preparation method of vitamin A microcapsule rice flour nutrition intensifier |
| CN110693848A (en) * | 2019-10-26 | 2020-01-17 | 大连医诺生物股份有限公司 | Vitamin A microcapsule preparation without antioxidant and preparation method thereof |
| CN113785987A (en) * | 2021-09-14 | 2021-12-14 | 万华化学集团股份有限公司 | Preparation method of vitamin A microcapsule |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103976353A (en) * | 2014-04-24 | 2014-08-13 | 武汉星辰现代生物工程有限公司 | Beta-carotene microcapsule production method |
| CN103976353B (en) * | 2014-04-24 | 2016-05-11 | 武汉星辰现代生物工程有限公司 | A kind of production method of beta carotene microcapsules |
| CN104522681A (en) * | 2015-01-10 | 2015-04-22 | 黄家亨 | Vitamin A absorption promoter and corresponding vitamin A replenisher comprising same |
| CN104522681B (en) * | 2015-01-10 | 2016-08-24 | 漯河医学高等专科学校 | A kind of vitamin A absorption accelerator and corresponding vitamin A supplement thereof |
| CN105456235A (en) * | 2015-11-20 | 2016-04-06 | 厦门金达威维生素有限公司 | High-stability and high-potency-unit vitamin A oil and preparation method thereof |
| CN105456235B (en) * | 2015-11-20 | 2019-03-29 | 厦门金达威维生素有限公司 | A kind of high unit vitamin A finish of high stability and preparation method thereof |
| CN106579407A (en) * | 2016-12-02 | 2017-04-26 | 南通励成生物工程有限公司 | Preparation method of vitamin A microcapsule rice flour nutrition intensifier |
| CN106579407B (en) * | 2016-12-02 | 2020-10-20 | 南通励成生物工程有限公司 | Preparation method of vitamin A microcapsule rice flour nutrition enhancer |
| CN110693848A (en) * | 2019-10-26 | 2020-01-17 | 大连医诺生物股份有限公司 | Vitamin A microcapsule preparation without antioxidant and preparation method thereof |
| CN110693848B (en) * | 2019-10-26 | 2021-12-14 | 大连医诺生物股份有限公司 | Vitamin A microcapsule preparation without antioxidant and preparation method thereof |
| CN113785987A (en) * | 2021-09-14 | 2021-12-14 | 万华化学集团股份有限公司 | Preparation method of vitamin A microcapsule |
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Address after: 361004 Fujian County of Yongchun Province town of peach Tao Xi Cun Quanzhou Ryan Biochemical Co. Ltd. Applicant after: He Dehai Address before: Xiamen City, Fujian province 361004 Wo Road, Siming District of Xiamen No. 819 Applicant before: He Dehai |
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Application publication date: 20110928 |