CN101444495B - Vitamin E microcapsule preparation method - Google Patents
Vitamin E microcapsule preparation method Download PDFInfo
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- CN101444495B CN101444495B CN2008102426713A CN200810242671A CN101444495B CN 101444495 B CN101444495 B CN 101444495B CN 2008102426713 A CN2008102426713 A CN 2008102426713A CN 200810242671 A CN200810242671 A CN 200810242671A CN 101444495 B CN101444495 B CN 101444495B
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Abstract
A vitamin E microcapsule preparation method belongs to the technical field of preparation of controlled-release microcapsule for food additives and bioactive substances. The vitamin E microcapsule preparation method can improve the stability of vitamin E and amplify the application range. The method comprises the following steps: selecting chitosan and maltodextrin as wall material, selecting soybean lecithin (P powder) and Tween-80 as the composite emulsifying agent; and synthesizing vitamin E microcapsule by spray drying. The vitamin E microcapsule has embedding rate up to 92.45%, retention rate up to 91.73%, and water content lower than 3%, and has wide application prospect in the fields of bread or snack products, beverages, biscuits, health products and nutrient fortified food, etc. The method has the advantage of low cost and simple process, can meet the environmental protection and practical requirement.
Description
Technical field
A kind of preparation method of Vitamin E contained micro capsule belongs to the microcapsule preparing technical field of food additive and bioactive substance sustained release.
Background technology
Vitamin E is a class nutritional labeling of needed by human; it is a kind of strong effectively free radical scavenger; can protect body cell film and life macromolecule to exempt from the attack of free radical; be the Natural antioxidant of a class highly effective and safe, at slow down aging, prevent and treat cardiovascular disease, anti-tumor aspect has good effect.No matter natural Vitamin E still on safety all is better than synthesising complex E at nutrition, physiologically active.Along with going deep into of threpsology and pathological research, the how new function of vitamin E is found constantly and is confirmed that people are increasing to the demand of vitamin E, and its effect more and more is subject to people's attention.
Vitamin E belongs to oil-soluble heat-sensitive materials, be difficult to water-soluble substances miscible, make it be difficult to add to uniformly in the water solublity food product, and ultraviolet, alkali and oxygen etc. can both destroy vitamin E, so will seal usually, keep in Dark Place, limit the application of vitamin E so greatly in food industry.Microcapsule technology is to protect core to avoid adverse environmental factors such as influences such as light, oxygen with filmogen embedding solid, liquid or gas; improve the stability and the shelf life of product with this; the range of application of expansion core, and a kind of technology of control core release.It can change physical form, protect sensitive composition, isolate active substance, reduce volatility, make immiscible composition mix and reduce the toxicity of some chemical addition agent, the application of having succeeded in many fields such as food, chemical industry, medicine, biotechnology.In food industry, manyly, technology barrier is achieved by microcapsule technology owing to can not get development product, and make the quality of traditional product be greatly improved, for the exploitation of food industry new and high technology has represented good prospect.Vitamin E is made the micro encapsulation vitamin E with methods such as spray dryinges, can keep the intrinsic property of vitamin E, can overcome its easy oxidation and water-fast shortcoming again.The Vitamin E contained micro capsule product can be used for bread or aspects such as snack food product, beverage, Biscuits, health food and nourishing reinforced food, has broad application prospects.
A lot of researchs about Vitamin E contained micro capsule have been arranged both at home and abroad.Patent publication No. is CN1927188A, invent a kind of preparation method of voltage endurance vitamin E microcapsule, 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%, the mechanical strength of gained microcapsule is enough to satisfy the tabletting requirement, and fuel load can be up to 70%.Patent publication No. is CN1568969A, invent a kind of preparation method and purposes of vitamin E clathrate, by cyclodextrin or cyclodextrin derivative vitamin E is carried out enclose, preferred HP-, the content of vitamin E of the enclose material of gained is below 10%.The above patent of comparing, the present invention with wide material sources, chitosan with low cost and maltodextrin as the wall material, do not add auxiliary capsule material, adopt biphase emulsion process, prepare the Vitamin E contained micro capsule product by spray-dired method, technology is simple, helps large-scale industrial production, and the vitamin E carrying capacity is greater than 30%.Complex coacervation also is a kind of means of Vitamin E contained micro capsuleization in addition, but the used common cost of wall material is higher, the complexity that technology also compares, and used cross-linking agent is also often toxic.Cross-linking method also is a kind of method of Vitamin E contained micro capsuleization, and at present, external having much prepares fatsoluble vitamin microcapsule patent with cross-linking method, but the method technology is comparatively complicated, and cross-linking process needs Consideration more, and this method is also being updated.Along with microcapsule research deepens continuously, it is also more and more to can be used for the Vitamin E contained micro capsule method, but spray drying method is still most popular method at present.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of process safety Vitamin E contained micro capsule simple, with low cost, improve the stability of vitamin E, control its dispose procedure, enlarge the scope of its application.
Technical scheme of the present invention: with the vitamin E is core, with chitosan and maltodextrin is the wall material, is compound emulsifying agent with soybean lecithin and Tween-80, by high-pressure emulsification and centrifugal spray drying technology, prepare pulverous Vitamin E contained micro capsule product, preparation process is as follows:
(1) chitosan is dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 1.5%～2.25% clear solution;
(2) maltodextrin is dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 37.5%～50% solution;
(3) soybean lecithin and Tween-80 are dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0 according to 4: 2 mass ratio as compound emulsifying agent, forming mass fraction is 1.5%～1.75% composite emulsifying agent solution;
(4) vitamin E is added in the composite emulsifying agent solution that step (3) obtains according to the mass ratio with compound emulsifying agent 1: 0.25～0.35, stirring (700～1000rpm) time uniform core emulsions of formation;
(5) with the chitosan solution of step (1), be added to while stirring in the core emulsion that step (4) obtains, high speed shear emulsifying again (10000～13000rpm, 3～5min) obtain the elementary emulsion of microcapsule;
(6) maltodextrin solution of step (2) is added to while stirring in the elementary emulsion of microcapsule that step (5) obtains, and high speed shear emulsifying again (10000～13000rpm, 3～5min) obtain final microcapsule emulsion; Control that the related component mass percent is in the final microcapsule emulsion: vitamin E 5%～6.5%, chitosan 0.4%～0.6%, maltodextrin 15%～20% and compound emulsifying agent 1.5%～1.75%;
(7) with the microcapsule emulsion of step (6) gained, through 40～50MPa, homogenizing 3 times carries out spray drying then, promptly gets the Vitamin E contained micro capsule powder.The spray drying parameter is: 180 ℃ of intake air temperatures, and 80 ℃ of air outlet temperature, charging under the room temperature, flow velocity is 1～2L/h.
The deacetylation of used chitosan is 80%～85%.
The DE value of used maltodextrin is between 15 to 20.
Used soybean lecithin is Powdered, and acetone insoluble matter wherein is 97%, and HLB is 7.
Used vitamin E is a natural Vitamin E, its total tocopherol content 〉=90%.
Beneficial effect of the present invention: the Vitamin E contained micro capsule that adopts said method to make, its characteristics are: vitamin E is added in the compound emulsion agent solution, after high-speed stirred, emulsifying agent can be distributed on the surface of vitamin E rapidly, when adding chitosan solution, because under acid condition, the chitosan molecule surface has a large amount of positive charges, under electrostatic effect, chitosan molecule can be adsorbed the surface that is dispersed in vitamin E, when adding maltodextrin solution again, be equivalent to vitamin E oil has been carried out secondary embedding, play the effect of wrapping up and filling out envelope, and in whole embedding process, because it is more stable that vitamin E is under the acid condition, the loss of vitamin E seldom in therefore producing.
The preparation method of Vitamin E contained micro capsule provided by the invention is with low cost, technology simple, meet environmental protection and practical requirement.Used chitosan, wide material sources and cheap, it has unique physiology and chemical characteristic simultaneously, nontoxic, excellent biological compatibility, biodegradability arranged, it is a kind of good biomaterial, having good film property again, is a kind of ideal microcapsule wall material, and same used maltodextrin also is cost-effective wall material.Used emulsifying agent soybean lecithin and Tween-80 do not have toxicity to human body, and soybean lecithin has very high nutritive value, and wide material sources, cheap.Vitamin E behind the micro encapsulation can keep the intrinsic property of vitamin E, can overcome its easy oxidation and water-fast shortcoming again.The Vitamin E contained micro capsule of gained of the present invention, embedding rate can reach more than 90%, retention rate also can reach more than 90% and the moisture of product below 3%, it can be used for bread or aspects such as snack food product, beverage, Biscuits, health food and nourishing reinforced food, has broad application prospects.
Specific embodiments
Embodiment 1: the preparation method of Vitamin E contained micro capsule, it comprises the steps:
(1) take by weighing the 2.4g chitosan and be dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 1.5% clear solution;
(2) take by weighing the 120g maltodextrin and be dissolved in acetic acid-sodium acetate buffer, the formation mass fraction is 50% solution;
(3) take by weighing the 6g soybean lecithin and 3g Tween-80 is dissolved in buffer as compound emulsifying agent, forming mass fraction is 1.5% composite emulsifying agent solution;
(4) take by weighing the 30g vitamin E oil and add in the composite emulsifying agent solution that step (3) obtains, the mass ratio of compound emulsifying agent and vitamin E oil is 0.3: 1, is stirring (700～1000rpm) time uniform core emulsions of formation;
(5) with 1.5% chitosan solution of step (1), be added to while stirring in the core emulsion that step (4) obtains, high speed shear emulsifying again (10000～13000rpm, 3～5min) obtain the elementary emulsion of microcapsule;
(6) 50% maltodextrin solution of step (2) is added to while stirring in the elementary emulsion of microcapsule that step (5) obtains, and high speed shear emulsifying again (10000～13000rpm, 3～5min) obtain final microcapsule emulsion;
(7) with the microcapsule emulsion of step (6) gained, through 40～50MPa, homogenizing 3 times carries out spray drying then, and the inlet temperature of spray dryer is that 180 ℃, outlet temperature are 80 ℃, charging under the room temperature, and the feed liquid flow velocity is 1～2L/h.
The microcapsule product of gained is creamy white, and has color and luster preferably, and embedding rate is 92.45%, and retention rate is 85.88%, and moisture is 2.34%.
Embodiment 2: the preparation method of vitamin E oil microcapsule, it comprises the steps:
(1) take by weighing the 3.6g chitosan and be dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 2.25% clear solution.
(2) take by weighing the 90g maltodextrin and be dissolved in acetic acid-sodium acetate buffer, the formation mass fraction is 37.5% solution.
(3) take by weighing the 7g soybean lecithin and 3.5g Tween-80 is dissolved in buffer as compound emulsifying agent, forming mass fraction is 1.75% composite emulsifying agent solution.
(4) take by weighing the 30g vitamin E oil and add in the composite emulsifying agent solution that step (3) obtains, the mass ratio of compound emulsifying agent and vitamin E oil is 0.35: 1, and (700～1000rpm) form uniform core emulsion stirring.
(5) with 2.25% chitosan solution of step (1), be added to while stirring in the core emulsion that step (4) obtains, (10000～13000rpm, 3～5min) obtain the elementary emulsion of microcapsule in high speed shear emulsifying again.
(6) 37.5% maltodextrin solution of step (2) is added to while stirring in the elementary emulsion of microcapsule that step (5) obtains, (10000～13000rpm, 3～5min) obtain final microcapsule emulsion in high speed shear emulsifying again.
(7) with the microcapsule emulsion of step (6) gained, through 40～50MPa, homogenizing 3 times carries out spray drying then, and the inlet temperature of spray dryer is that 180 ℃, outlet temperature are 80 ℃, charging under the room temperature, and the feed liquid flow velocity is 1～2L/h.
The microcapsule product of gained is creamy white, and has color and luster preferably, and embedding rate is 79.64%, and is expected to surpass 80%, and retention rate is 89.90%, and moisture is 2.38%.
Embodiment 3: the preparation method of vitamin E oil microcapsule, it comprises the steps:
(1) take by weighing the 3.6g chitosan and be dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 2.25% clear solution.
(2) take by weighing the 120g maltodextrin and be dissolved in acetic acid-sodium acetate buffer, the formation mass fraction is 50% solution.
(3) take by weighing 6.5g soybean lecithin and 3.25gTween-80 and be dissolved in buffer as compound emulsifying agent, forming mass fraction is 1.625% composite emulsifying agent solution.
(4) take by weighing the 39g vitamin E oil and add in the composite emulsifying agent solution that step (3) obtains, the mass ratio of compound emulsifying agent and vitamin E oil is 0.25: I, (700～1000rpm) form uniform core emulsion stirring.
(5) with 2.25% chitosan solution of step (1), be added to while stirring in the core emulsion that step (4) obtains, (10000～13000rpm, 3～5min) obtain the elementary emulsion of microcapsule in high speed shear emulsifying again.
(6) 50% maltodextrin solution of step (2) is added to while stirring in the elementary emulsion of microcapsule that step (5) obtains, (10000～13000rpm, 3～5min) obtain final microcapsule emulsion in high speed shear emulsifying again.
(7) with the microcapsule emulsion of step (6) gained, through 40～50MPa, homogenizing 3 times carries out spray drying then, and the inlet temperature of spray dryer is that 180 ℃, outlet temperature are 80 ℃, charging under the room temperature, and the feed liquid flow velocity is 1～2L/h.
The microcapsule product of gained is creamy white, and has color and luster preferably, and embedding rate is 89.02%, and is expected to surpass 90%, and retention rate is 91.73%, and moisture is 2.67%.
Claims (6)
1. the preparation method of a Vitamin E contained micro capsule, it is characterized in that with the vitamin E being core, with chitosan and maltodextrin is the wall material, with soybean lecithin and Tween-80 is compound emulsifying agent, by high-pressure emulsification and centrifugal spray drying technology, prepare pulverous Vitamin E contained micro capsule product, preparation process is as follows:
(1) chitosan is dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 1.5%～2.25% transparent chitosan solution;
(2) maltodextrin is dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0, the formation mass fraction is 37.5%～50% maltodextrin solution;
(3) soybean lecithin and Tween-80 are dissolved in the acetic acid-sodium acetate buffer of 0.1mol/L, pH3.0～4.0 according to 4: 2 mass ratio as compound emulsifying agent, forming mass fraction is 1.5%～1.75% composite emulsifying agent solution;
(4) vitamin E oil is added in the composite emulsifying agent solution that step (3) obtains according to the mass ratio with compound emulsifying agent 1: 0.25～0.35, under 700～1000rpm stirs, form uniform core emulsion;
(5) with the chitosan solution of step (1), be added to while stirring in the core emulsion that step (4) obtains, 10000～13000rpm, the emulsifying of 3～5min high speed shear obtain the elementary emulsion of microcapsule again;
(6) maltodextrin solution of step (2) is added to while stirring in the elementary emulsion of microcapsule that step (5) obtains, 10000～13000rpm, the emulsifying of 3～5min high speed shear obtain final microcapsule emulsion again; Control that the related component mass percent is in the final microcapsule emulsion: vitamin E 5%～6.5%, chitosan 0.4%～0.6%, maltodextrin 15%～20% and compound emulsifying agent 1.5%～1.75%;
(7) with the microcapsule emulsion of step (6) gained,, carry out spray drying then, promptly get the Vitamin E contained micro capsule powder through 40～50MPa high pressure homogenize.
2. preparation method according to claim 1, the deacetylation that it is characterized in that used chitosan is 80%～85%.
3. preparation method according to claim 1, the DE value that it is characterized in that used maltodextrin is between 15 to 20.
4. preparation method according to claim 1 is characterized in that used soybean lecithin is Powdered, and acetone insoluble matter wherein is 97%, and HLB is 7.
5. preparation method according to claim 1 is characterized in that used vitamin E is a natural Vitamin E, its total tocopherol content 〉=90%.
6. preparation method according to claim 1 is characterized in that microcapsule emulsion homogenizing 3 times under 40～50MPa; The spray drying parameter is: intake air temperature is that 180 ℃, air outlet temperature are that charging under 80 ℃, room temperature, flow velocity are 1～2L/h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101972619A (en) * | 2010-09-01 | 2011-02-16 | 浙江中烟工业有限责任公司 | Preparation method of menthol microcapsules |
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| CN1879609A (en) * | 2006-05-10 | 2006-12-20 | 浙江大学 | A method for preparing silk fibroin Vitamin E contained micro capsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1879609A (en) * | 2006-05-10 | 2006-12-20 | 浙江大学 | A method for preparing silk fibroin Vitamin E contained micro capsule |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101972619A (en) * | 2010-09-01 | 2011-02-16 | 浙江中烟工业有限责任公司 | Preparation method of menthol microcapsules |
| CN101972619B (en) * | 2010-09-01 | 2012-05-23 | 浙江中烟工业有限责任公司 | Preparation method of menthol microcapsules |
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Assignee: Guangdong comfort Pharmaceutical Co. Ltd. Assignor: Jiangnan University Contract record no.: 2011320010098 Denomination of invention: Vitamin E microcapsule preparation method Granted publication date: 20100609 License type: Exclusive License Open date: 20090603 Record date: 20110719 |
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