CN103054030A - Method for preparing perilla oil powder through microencapsulation - Google Patents
Method for preparing perilla oil powder through microencapsulation Download PDFInfo
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- CN103054030A CN103054030A CN2013100316809A CN201310031680A CN103054030A CN 103054030 A CN103054030 A CN 103054030A CN 2013100316809 A CN2013100316809 A CN 2013100316809A CN 201310031680 A CN201310031680 A CN 201310031680A CN 103054030 A CN103054030 A CN 103054030A
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Abstract
The invention discloses a method for preparing perilla oil powder through microencapsulation, and provides a method for preparing perilla oil powder with simple technology and good water solubility. The method comprises the following steps of: heating to gelatinize starch octenylsuccinate at 90-100 DEG C, and cooling to room temperature; preparing the gelatinized starch octenylsuccinate into an aqueous solution of starch octenylsuccinate with mass concentration of 30-40%; adding perilla oil into the aqueous solution of starch octenylsuccinate, and stirring for emulsification at high temperature to obtain an emulsion; and homogenizing the emulsion, and spray-drying to obtain perilla oil powder. The preparation method disclosed by the invention adopts starch octenylsuccinate as a wall material, does not need addition of an emulsifier and realizes high embedding rate; the operation technology is simple; and the perilla oil powder has good water solubility, good dispersity and good stability. Moreover, the starch octenylsuccinate has low price, the product cost can be lowered, and the product popularization is facilitated.
Description
Technical field
The present invention relates to food processing technology field, particularly relate to the method that a kind of microencapsulation prepares perilla oil powder.
Background technology
(Perilla frutescens) is widely distributed in China for purple perilla, is the traditional medicine food dual purpose plant of China, also be health ministry first batch of promulgate be food be again one of 60 kinds of article of medicine.The purple perilla seed is rich in vegetable oil, and the perilla herb oil that extracts from the purple perilla seed can obviously suppress the incidence of disease of breast cancer due to the dimethylbenzanthracene, has reducing blood lipid, brain tonic and improves learning memory, anti-senescence function and anti-allergic effects.Alpha-linolenic acid content can up to 54%-64%, be higher than other vegetable oil far away in the perilla herb oil.Leukotrienes is one of essential fatty acid, but metabolism is EPA and DHA(plant docosapentaenoic acid in human body), do not contain cholesterol, but for a long time generation of edible angiocardiopathy preventing is of value to healthy.And perilla herb oil is harmless, without the stink of fish oil, the delicate fragrance of vegetable oil has remedied again the deficiency of fish oil fishy smell, two keys are corresponding less, stability is better than fish oil, thereby perilla herb oil is described as the land deep sea fish oil, has important nutrition health-care functions and huge exploitation is worth.
Perilla herb oil is the sensitive materials that a class very easily is subjected to such environmental effects, and is very easy oxidized, is difficult to long term storage, product range of application relative narrower.The form of perilla herb oil product is more single, mainly is the product appearance with the fluid oil form.In addition, also having a small amount of perilla herb oil to be made into soft capsule uses as health products.
Along with the continuous progress of technology, the method for preparing perilla herb oil by microencapsulation becomes the direction of research gradually.Give the good flowability of product, dispersiveness, the characteristic such as water-disintegrable and stable with the perilla herb oil microencapsulation, preferably resolve perilla herb oil and carry inconvenience, range of application is narrow, the product shelf phase is short problem.It is that compound wall materials carries out embedding to perilla herb oil that prior art such as patent application CN200810046897.6 adopt protein and polysaccharide, but protein poorly water-soluble, especially near easily cohesion isoelectric point, meet the characteristics of hot and cold mutability, when preparation perilla herb oil microcapsules, control to experiment condition is comparatively strict, complex process.
Summary of the invention
The objective of the invention is for the technological deficiency that exists in the prior art, and provide a kind of technique simple, good water solubility, the microencapsulation of stable in properties prepares the method for perilla oil powder.
For realizing that the technical scheme that purpose of the present invention adopts is:
A kind of microencapsulation prepares the method for perilla oil powder, comprises the steps:
(1) 90～100 ℃ of lower heating gelatinization starch octenyl succinate anhydride is cooled to room temperature;
(2) starch octenyl succinate anhydride after the gelatinization being made mass concentration is 30～40% the starch octenyl succinate anhydride aqueous solution;
(3) add perilla herb oil in the above-mentioned starch octenyl succinate anhydride aqueous solution, high-temperature stirring emulsification obtains emulsion; Wherein, the mass ratio of described starch octenyl succinate anhydride and perilla herb oil is 5:1;
(4) the emulsion homogeneous that step (3) is obtained obtains the emulsion of stable homogeneous;
(5) the emulsion spray drying behind the above-mentioned homogeneous is obtained perilla oil powder.
Homogeneous is with the speed homogeneous 2min of 13000r/min in the step (4).
High-temperature stirring in the described step (3) is to stir at 60 ℃ of lower magnetic forces.
EAT during spray drying treatment is 190 ℃, and leaving air temp is 100 ℃, and feed rate is 55mL/min.
Compared with prior art, the invention has the beneficial effects as follows:
1, to adopt starch octenyl succinate anhydride be the wall material to preparation method of the present invention, and starch octenyl succinate anhydride has good emulsibility, film forming, thickening property and water-soluble, uses as microcapsule wall material, need not to add emulsifying agent, and technique is simple.
2, preparation method's embedding rate of the present invention is high: it is the wall material that preparation method of the present invention adopts starch octenyl succinate anhydride, starch octenyl succinate anhydride has certain emulsifying capacity, can the oil-water interfaces of emulsion form one deck tough and tensile, larger cohesive force, continuously and the film that is difficult for breaking arranged, so that dispersion particle is coalescent and separate all relatively difficulty, thereby reach the effect of stable emulsion.And viscosity still can keep very low during high solid content, therefore, can suitably increase solid content, rapidly dehydration evaporation in spray-drying process, film forming speed is fast, reduce the loss of core, be conducive to the formation of cyst wall in the spray-drying process and the raising of cyst wall density, thereby improved embedding rate.
3, preparation method of the present invention utilizes starch octenyl succinate anhydride embedding perilla herb oil, and operating procedure is easy, and the starch octenyl succinate anhydride price is low, can reduce the cost of product, is conducive to the popularization of product.
4, preparation method of the present invention utilizes starch octenyl succinate anhydride embedding perilla herb oil, and this wall material has good water-soluble and stable, thereby gives perilla oil powder good water-soluble, dispersed, stable, has greatly widened the application of perilla herb oil.
5, preparation method of the present invention utilizes starch octenyl succinate anhydride embedding perilla herb oil, this wall material has good stability in acid, alkaline environment, operating condition is easy to control in the preparation process, and the microcapsule product stable in properties of gained effectively prolongs shelf-life of perilla herb oil.
6, preparation method of the present invention adopts 60 ℃ of emulsifying temperatures, and with the 13000r/min high speed homogenization, is conducive to like this contacting of lipophilic group in grease and the wall material, and affinity increases, and obtains highly uniform and stable emulsion, thereby guarantees efficient embedding perilla herb oil.
7, the emulsion rapid spray drying treatment of preparation method of the present invention after with emulsifying homogeneous obtains microcapsule product, can guarantee like this emulsion drying and moulding under the most stable state of gained, can guarantee feed temperature again.Emulsion viscosity and flowability under this temperature are optimum state, and its feed liquid in spray-drying process is fully atomized, and the specific area that contacts with hot-air increases, and evaporation and cyst wall fast filming solidify rapidly to be conducive to moisture.
8, preparation method of the present invention adopts spray drying process to prepare the perilla herb oil microcapsules, EAT during spray drying treatment is 190 ℃, leaving air temp is 100 ℃, feed rate is 55mL/min, can form rapidly the smooth microcapsule structure of complete densification with this understanding, products obtained therefrom moisture content low (below 5%) has good free-running property.
Description of drawings
Figure 1 shows that starch octenyl succinate anhydride embedding perilla herb oil microcapsules amplify 1000 times stereoscan photograph;
Figure 2 shows that starch octenyl succinate anhydride embedding perilla herb oil microcapsules amplify 5000 times stereoscan photograph.
Figure 3 shows that under the condition of 65 ° of C the situation of change of perilla herb oil microcapsules and perilla herb oil peroxide value in storage process.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment 1
(1) nearly boiling water (90～100 ℃) water-bath gelatinization starch octenyl succinate anhydride 10min naturally cools to room temperature.
(2) starch octenyl succinate anhydride after the gelatinization being made mass concentration is 30% the starch octenyl succinate anhydride aqueous solution.
(3) in the above-mentioned starch octenyl succinate anhydride aqueous solution, press the core wall than for 1:5 adds perilla herb oil, afterwards, stir at 60 ℃ of lower magnetic forces, obtain emulsion.
(4) emulsion that step (3) is obtained obtains the emulsion of stable homogeneous with the speed homogeneous 2min of 13000r/min.
(5) the rapid spray-drying of the emulsion behind the above-mentioned homogeneous is obtained perilla oil powder, the EAT during spray drying treatment is 190 ℃, and leaving air temp is 100 ℃, and feed rate is 55mL/min.
The stereoscan photograph of the present embodiment products obtained therefrom can find out from Fig. 1,2 as shown in Figure 1, 2, and the perilla herb oil microcapsules are observed under ESEM and shown capsule particle rounding, smooth surface, compact structure, flawless and breakage.The embedding quality that this product is described is good, but long term storage.The capsule particle diameter mainly is distributed between the 2-16 μ m.
Other performance tests of the present embodiment products obtained therefrom are as follows:
1, being determined as follows of microscapsule powder embedding rate: accurately take by weighing the microcapsule product of 2g embodiment 1 gained, put into the funnel of filter paper, with 50mL petroleum ether sample, collect cleaning solution, reclaim benzinum, weigh to such an extent that surface oil is heavy.
The quality 1.9971g of sample, the quality 21.4083g of bottle, the quality 21.4125g of bottle behind the recovery benzinum
Surface oil content (%)=surface oil weight/sample weight * 100=(21.4125-21.4083)/1.9971 * 100=0.2103
Microcapsules sample (m with the embodiment 1 that accurately weighs
1) to dry triangular flask, add 20mL hot water, sample is fully dissolved after, add after the 20mL benzinum fully extracts, extract is moved into (m in the triangular flask of having weighed
2), re-extract twice, combining extraction liquid is sloughed solvent under 30 ℃, put into 60 ℃ of baking ovens (m that dries to constant weight again
3), calculate total oil content:
m
1=5.0003g,m
2=46.5875g,m
3=47.5020g
Total oil content=(m
3-m
2)/m
1=(47.5020-46.5875)/5.0003=18.29%
Microencapsulation efficient (%)=(1-surface oil content/product oil content) * 100=(1-0.2103%/18.29%) * 100=98.85
Can be found out by surface oil content and microencapsulation efficient, the perilla herb oil major part is embedded in the wall material particle, is exposed to the perilla herb oil content of surface of microcapsule seldom, and the embedding effect is remarkable.
2, being determined as follows of the storage-stable of microcapsule product: at the bottom of the product of spray-drying preparation and the perilla herb oil of embedding not be layered on conical flask equably, put into 65 ℃ of accelerated oxidation tests of carrying out grease of insulating box, survey a peroxide value every 24h, the result as shown in Figure 3.As can be seen from Figure 3, prolongation along with standing time, the peroxide value of perilla herb oil crude oil increases rapidly, accompany irritant rancidity, peroxide value then slightly rises behind the perilla herb oil microencapsulation, and stability is far superior to perilla herb oil, illustrate that spray drying process embedding perilla herb oil can effectively reduce contacting of perilla herb oil and external environment, suppress the generation of perilla herb oil redox reaction, thereby improved the stability of perilla herb oil, reached the purpose that prolongs the perilla herb oil shelf-life.
3, the instant capacity of microscapsule powder and dispersed assay method are as follows: the microscapsule powder of a little embodiment 1 is put into cup, pour temperature and be 50 ℃ distilled water, stirring, microscapsule powder fully is dissolved in rapidly in 50 ℃ of hot water in the rear observation cup, the solution that obtains is that milky is translucent, no suspended substance, floccule and lamination.Still can keep stable after long-time the placement.
Embodiment 2
(1) nearly boiling water (90～100 ℃) water-bath gelatinization starch octenyl succinate anhydride 10min naturally cools to room temperature.
(2) starch octenyl succinate anhydride after the gelatinization being made mass concentration is 40% the starch octenyl succinate anhydride aqueous solution.
(3) in the above-mentioned starch octenyl succinate anhydride aqueous solution, press the core wall than for 1:5 adds perilla herb oil, afterwards, stir at 60 ℃ of lower magnetic forces, obtain emulsion.
(4) emulsion that step (3) is obtained obtains the emulsion of stable homogeneous with the speed homogeneous 2min of 13000r/min.
(5) the emulsion spray drying behind the above-mentioned homogeneous is obtained perilla oil powder, the EAT during spray drying treatment is 190 ℃, and leaving air temp is 100 ℃, and feed rate is 55mL/min.
The perilla herb oil microcapsule product of embodiment 2 gained is observed under ESEM and is shown to have the particle rounding, smooth surface, and compact structure, flawless and breakage, the embedding quality is good, but long term storage.
The present invention utilizes starch octenyl succinate anhydride embedding perilla herb oil, the perilla herb oil microcapsules of preparation overcome oxidative rancidity, range of application that perilla herb oil causes because unsaturated fatty acid content is high narrow, carry the shortcomings such as inconvenient, have fabulous storage-stable, take convenience, stable in properties, be of high nutritive value.And technique is simple, and embedding rate is high.
The above only is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a microencapsulation prepares the method for perilla oil powder, it is characterized in that, comprises the steps:
(1) 90～100 ℃ of lower heating gelatinization starch octenyl succinate anhydride is cooled to room temperature;
(2) starch octenyl succinate anhydride after the gelatinization being made mass concentration is 30～40% the starch octenyl succinate anhydride aqueous solution;
(3) add perilla herb oil in the above-mentioned starch octenyl succinate anhydride aqueous solution, high-temperature stirring emulsification obtains emulsion; Wherein, the mass ratio of described starch octenyl succinate anhydride and perilla herb oil is 5:1;
(4) the emulsion homogeneous that step (3) is obtained obtains the emulsion of stable homogeneous;
(5) the emulsion spray drying behind the above-mentioned homogeneous is obtained perilla oil powder.
2. microencapsulation according to claim 1 prepares the method for perilla oil powder, it is characterized in that, homogeneous is with the speed homogeneous 2min of 13000r/min in the step (4).
3. microencapsulation according to claim 1 prepares the method for perilla oil powder, it is characterized in that, the high-temperature stirring in the described step (3) is to stir at 60 ℃ of lower magnetic forces.
4. microencapsulation according to claim 1 prepares the method for perilla oil powder, it is characterized in that, the EAT during the dry processing of emulsion spray is 190 ℃, and leaving air temp is 100 ℃, and feed rate is 55mL/min.
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Cited By (19)
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| CN103349785A (en) * | 2013-07-26 | 2013-10-16 | 广东省中医药工程技术研究院 | Traditional Chinese medicine volatile oil complex and preparation method thereof |
| CN103416757A (en) * | 2013-09-06 | 2013-12-04 | 贵州大学 | Dendrocalamus oil microcapsule and preparation method thereof |
| CN103519178A (en) * | 2013-10-25 | 2014-01-22 | 天津商业大学 | Preparation method of ginseng nano-microcapsule |
| CN103564065A (en) * | 2013-10-30 | 2014-02-12 | 广州绿萃生物科技有限公司 | Preparation method of purple perilla seed oil microcapsule |
| CN103919140A (en) * | 2014-05-07 | 2014-07-16 | 河南工业大学 | Perilla oil microsphere and preparation method thereof |
| CN105077249A (en) * | 2015-09-06 | 2015-11-25 | 蓬莱海洋（山东）股份有限公司 | Conjugated linoleic acids capsule and preparation method thereof |
| CN105192102A (en) * | 2015-11-03 | 2015-12-30 | 东北农业大学 | Perilla frutescens oil microcapsule rich in beta-carotene and preparation method of perilla frutescens oil microcapsule |
| CN105995978A (en) * | 2016-05-20 | 2016-10-12 | 福建师范大学 | Perilla oil composition and perilla oil microcapsule powder and preparation method thereof |
| CN106343577A (en) * | 2015-07-09 | 2017-01-25 | 北京宝得瑞食品有限公司 | Water-soluble sea buckthron oil microcapsules with high oil carrying capacity and preparation method thereof |
| CN107188978A (en) * | 2017-07-04 | 2017-09-22 | 华南理工大学 | A kind of starch octenyl succinate anhydride and its preparation method and application |
| CN109907076A (en) * | 2019-03-29 | 2019-06-21 | 中北大学 | A kind of fire sesame slices essential oil microcapsule powder and its preparation method and application |
| CN110564503A (en) * | 2019-08-05 | 2019-12-13 | 中北大学 | Perilla essential oil microcapsule powder and preparation method and application thereof |
| CN110839894A (en) * | 2019-12-03 | 2020-02-28 | 郑州添之道食品科技有限公司 | Nutrient microcapsule and preparation method and application thereof |
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