CN103404854A - Preparation method of phytosterol ester microcapsules - Google Patents
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Abstract
The invention relates to a preparation method for phytosterol ester microcapsules, which comprises the following steps: firstly, taking Arabic gum and maltodextrin as wall materials, adding hydrophilic emulsifier, and dissolving by heating in a water bath, so as to prepare an aqueous phase wall material solution; then adding oleophylic emulsifier into phytosterol ester to prepare an oil phase core material solution; further, mixing the core material solution and the wall material solution under the ultrasonic-assisted condition, and emulsifying and homogenizing to acquire a homogeneous emulsion system; finally spray drying the emulsion, and screening to acquire powdery homogeneous phytosterol ester microcapsule products. The phytosterol ester microcapsule products prepared through the method have embedding rate more than 94%, solubility more than 95%, and fragrance; oxidation stability of the phytosterol ester is improved, and functional activity and nutrition of the phytosterol ester are favorably conserved; meanwhile, the method enables the phytosterol ester to transform from a liquid to a more stable solid, so that shelf life is prolonged, transportation and storage are facilitated, bioavailability of the phytosterol ester is improved, and the market demand is met more satisfactorily.
Description
Technical field
The invention belongs to grease deep processing technology field, be specifically related to a kind of preparation method of phytosterin ester microcapsules.
Background technology
Phytosterin ester is made by phytosterol and fatty acid esterification, because the chief component composition of phytosterol is cupreol, stigmasterol, brassicasterol and campesterol, so sterol ester mainly is comprised of cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester.Sterol ester can be absorbed by the body and be converted into sterol and aliphatic acid, and its specific ionization phytosterol has better Lowering cholesterol effect.Now be acknowledged as a kind of functional grease with health role, constantly be exploited in fields such as food, medicines.At present, phytosterin ester is mainly stored with the form transportation of bucket, because phytosterin ester is rich in unrighted acid, thereby very easily oxidative rancidity has reduced product quality, and it is water insoluble, is difficult to water-soluble substances miscible, be difficult to make an addition to equably in food, beverage, utilizability is lower.The limitation of phytosterin ester these self, greatly restricted its application in every field.
Microcapsules technology is that solid, liquid or gas are embedded in a kind of microencapsulation and form the technology with semi permeability or sealing cyst membrane.Microcapsules technology has the following advantages: the protection core, reduce the impact of external environment factor on it; Incompatible composition is mixed equably; The isolation active component, keep the original character of core, reduces the nutritive loss of component, extends storage period; Change physical behavior, convenient transportation, the expansion scope of application; Modification, the bad smell of covering core, color and luster etc.
The method of microencapsulation has a variety of, and wherein spray drying process is short because of its time, and cost is low, and technique is simple, is applicable to the large production of continuous and automatic, so be most widely used, is the main method of current commodity production and application.Spray drying process is best suited for the microencapsulation of lipophile material, and the lipophile of core is stronger, and the embedding effect is better.The key of microcapsule product quality and stability is screening, emulsification and the drying process with atomizing of wall material, and due to the condition difference, the microcapsule product quality made is also different.
At present the research of microencapsulation of phytosterol esters is reported seldom both at home and abroad, the research for application and development of microencapsulation of phytosterol esters also is in and has just started starting and exploratory stage.The application of phytosterin ester in the liquid foods such as beverage, milk of oily still has been subject to greatly restriction.Up to now, the phytosterin ester microcapsules are not also put in production practices and are gone on a large scale, and its industrialization and market application are also immature.
Summary of the invention
In order to improve the oxidation stability of phytosterin ester, improve product quality, be convenient to the transportation storage, improve its bioavilability, the invention provides a kind of preparation method of phytosterin ester microcapsules;
Concrete preparation manipulation step is as follows:
(1). the preparation of water phase wall material solution:
Get Arabic gum and be dissolved in the temperature 60 C deionized water, add maltodextrin to dissolve, at the temperature 60 C Water Under, bathe standing 30min, then add sucrose ester to mix, make water phase wall material solution; In water phase wall material solution, the mass fraction of Arabic gum is 4.13%～14.37%, and the mass fraction of maltodextrin is 3.44%～12.93%, and the mass fraction of sucrose ester is 0.8%～1.87%;
(2). the preparation of oil phase core material solution:
In phytosterin ester, add monoglyceride, mix, make oil phase core material solution; In oil phase core material solution, the mass fraction of phytosterin ester is 10.33%～21.56%, and the mass fraction of monoglyceride is 0.2%～0.47%;
(3). ultrasonic wave is auxiliary to be mixed:
Water phase wall material solution and oil phase core material solution are mixed under the water bath condition of temperature 60 C, the auxiliary 5min that stirs of ultrasonic wave, obtain mixed solution; In mixed solution, the mass ratio of oil phase core material solution and water phase wall material solution is 1:0.5～1:3;
(4). high-shear emulsifying:
In high-shear emulsion machine, mixed solution is carried out to emulsification, the shearing rotating speed is 10000r/min, and the time is 5min, obtains emulsion;
(5). high-pressure homogeneous:
By emulsion, at pressure, be under 20MPa～40MPa condition with high pressure homogenizer, homogeneous 2～4 times;
(6). spray-drying:
By the spray-drying under the air mass flow condition of the charging pump speed of 175 ℃ of the temperature～EAT of 195 ℃, the feeding temperature of temperature 60 C, 4.5ml/min～7.5ml/min, 350L/h～400L/h of the emulsion after homogeneous;
(7). screening:
The powder that spray-drying makes is crossed to 100 mesh sieves, obtain the phytosterin ester microcapsules, phytosterin ester microcapsule size homogeneous, have micro-sweet fragrant, and embedding rate is greater than 94%, and solubility is greater than 95%.
The percent value that reduced sugar in described maltodextrin (take glucose meter) accounts for the syrup dry is 15～20, and the hydrophilic hydrophobic balance value (HLB) of described sucrose ester is 15.
The hydrophilic hydrophobic balance value (HLB) of described monoglyceride is 3.8, in described phytosterin ester, contain cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester, the total content of cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester is greater than 98%.
The present invention with water miscible Arabic gum and maltodextrin as compound wall materials; monoglyceride and sucrose ester are as emulsifying agent; phytosterin ester is wrapped up, by spray-drying, make the water-soluble fine particle of sealing cyst membrane, phytosterin ester has been played to certain protective effect.With phytosterin ester, compare, the phytosterin ester microcapsules have water-soluble preferably, have farthest kept the activity of phytosterin ester functional components, improved the stability of product, improve the quality of product, be convenient to the transportation storage, enlarged its range of application.
Useful technique effect of the present invention embodies in the following areas:
1. the present invention adopts edible Arabic gum and maltodextrin as compound wall materials, reduced to a certain extent production cost, safety non-toxic, and Arabic gum has the function that reduces the cholesterol in blood, select Arabic gum can strengthen the effect of phytosterin ester microcapsules norcholesterol as the wall material, use it more to be of value to consumer's health;
2. the present invention utilizes the auxiliary mixing of ultrasonic wave, is conducive to accelerate mixing of core and wall material solution; In spray-drying process, control feeding temperature, reduced the viscosity of emulsion, strengthened the stability of emulsion, more be conducive to spray-dired carrying out;
3. the microcapsule embedded rate of phytosterin ester prepared of the present invention is greater than 94%, solubility is greater than 95%, can promptly in water, be dispersed into emulsion system equably, the microcapsule product profile is complete glassy state, seamless hole, density is high, can preserve preferably nutritional labeling and the biologically active of phytosterin ester, phytosterin ester and external environment are kept apart, prevent oxygen, the factors such as illumination are to its oxidative rancidity caused, oxidation stability and the Storage of phytosterin ester have been improved, be convenient to transportation, applicable to food, beverage, health products, dairy products, the aspects such as additive, widened the utilization rate of phytosterin ester,
4. technological operation of the present invention is simple and easy to do, and instrument and equipment requires low, is suitable for the automatic continuous large-scale production of factory, environment is not polluted environmental protection in operating process.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described.
In following examples, phytosterin ester is purchased from Shanghai and carrys out the sparrow bio tech ltd, in described phytosterin ester, contain cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester, the total content of cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester is 98%.
Arabic gum is purchased from the Shanghai sincere food selling of intelligent think of Co., Ltd, and maltodextrin is purchased from Shanghai western king's starch group, and percentage (DE) value that the reduced sugar of glucose meter of take in maltodextrin accounts for the syrup dry is 15～20.Sucrose ester is purchased from Liuzhou long-range food ingredient Science and Technology Ltd., and the hydrophilic hydrophobic balance value (HLB) of sucrose ester is 15, and monoglyceride is purchased from Huayang chemical industry Co., Ltd, and the hydrophilic hydrophobic balance value (HLB) of monoglyceride is 3.8.
EXAMPLE l:
The preparation method of phytosterin ester microcapsules is as follows:
1. the preparation of water phase wall material solution:
Take Arabic gum and be dissolved in temperature 60 C 500mL deionized water, add maltodextrin to dissolve, at the temperature 60 C Water Under, bathe standing 30min, then add sucrose ester to mix, make water phase wall material solution.In water phase wall material solution, the quality of Arabic gum is that its mass fraction of 32.33g(is 4.31%), the quality of maltodextrin is that its mass fraction of 48.53g(is 6.47%), the quality of sucrose ester is that its mass fraction of 6.00g(is 0.8%);
The mass fraction of each component=[each constituent mass/(total solid quality+solvent quality)] * 100%;
2, the preparation of oil phase core material solution:
In phytosterin ester, add monoglyceride, mix, make oil phase core material solution.In oil phase core material solution, the quality of phytosterin ester is that its mass fraction of 161.70g(is 21.56%), the quality of monoglyceride is that its mass fraction of 1.50g(is 0.2%);
3, ultrasonic wave is auxiliary mixes:
Water phase wall material solution and oil phase core material solution are mixed under the water bath condition of temperature 60 C, the auxiliary 5min that stirs of ultrasonic wave, obtain mixed solution.In mixed solution, the mass ratio of oil phase core material solution and water phase wall material solution is 1:0.5;
4, high-shear emulsifying:
By high-shear emulsion machine, prepared mixed solution is carried out to emulsification, the shearing rotating speed is 10000r/min, and the time is 5min, obtains emulsion;
5, high-pressure homogeneous:
By emulsion, at pressure, be under the 35MPa condition with high pressure homogenizer, homogeneous 2 times;
6, spray-drying:
By the spray-drying under the condition of 175 ℃ of EATs, 60 ℃ of feeding temperatures, 5 ml/min charging pump speeds, 350 L/h air mass flows of the emulsion after high-pressure homogeneous;
7, screening:
The powder that spray-drying makes is crossed to 100 mesh sieves, get final product to obtain the phytosterin ester microcapsule product.
Prepared phytosterin ester microcapsule product is faint yellow, and big or small homogeneous has micro-sweet fragrant, and embedding rate is 94.61%, and solubility is 95.86%.
Embodiment 2:
The preparation method of phytosterin ester microcapsules is as follows:
1. the preparation of water phase wall material solution:
Take in the 500mL deionized water that Arabic gum is dissolved in temperature 60 C, add maltodextrin to dissolve, at the temperature 60 C Water Under, bathe standing 30min, then add sucrose ester to mix, make water phase wall material solution.In water phase wall material solution, its mass fraction of quality 77.48g(of Arabic gum is 10.33%), the quality of maltodextrin is that its mass fraction of 77.48g(is 10.33%), the quality of sucrose ester is that its mass fraction of 14.03g(is 1.87%);
2, the preparation of oil phase core material solution:
In phytosterin ester, add monoglyceride, mix, make oil phase core material solution.In oil phase core material solution, the quality of phytosterin ester is that its mass fraction of 77.48g(is 10.33%), the quality of monoglyceride is that its mass fraction of 3.53g(is 0.47%);
3, ultrasonic wave is auxiliary mixes:
Water phase wall material solution and oil phase core material solution are mixed in the water bath condition of temperature 60 C, the auxiliary 5min that stirs of ultrasonic wave, obtain mixed solution.In mixed solution, the mass ratio of oil phase core material solution and water phase wall material solution is 1:2;
4, high-shear emulsifying:
By high-shear emulsion machine, resulting mixed solution is carried out to emulsification, the shearing rotating speed is 10000r/min, and the time is 5min, obtains emulsion;
5, high-pressure homogeneous:
By resulting emulsion, be under the 30MPa condition at pressure, homogeneous 3 times;
6, spray-drying:
By the spray-drying under the condition of 182 ℃ of EATs, 60 ℃ of feeding temperatures, 6.2 ml/min charging pump speeds, 370L/h air mass flow of the emulsion after high-pressure homogeneous;
7, screening:
The powder that spray-drying makes is crossed to 100 mesh sieves, get final product to obtain the phytosterin ester microcapsule product.
Prepared phytosterin ester microcapsule product is faint yellow, and big or small homogeneous has micro-sweet fragrant, and embedding rate is 97.87%, and solubility is 98.24%.
Embodiment 3:
The preparation method of phytosterin ester microcapsules is as follows:
1. the preparation of water phase wall material solution:
Take Arabic gum and be dissolved in temperature 60 C 500mL deionized water, add maltodextrin to dissolve, at the temperature 60 C Water Under, bathe standing 30min, then add sucrose ester to mix, make water phase wall material solution.In water phase wall material solution, the quality of Arabic gum is that its mass fraction of 36.98g(is 5.12%), the quality of maltodextrin is that its mass fraction of 83.21g(is 11.52%), the quality of sucrose ester is that its mass fraction of 7.73g(is 1.07%);
2, the preparation of oil phase core material solution:
Take phytosterin ester, then add monoglyceride, mix, make oil phase core material solution.In oil phase core material solution, the quality of phytosterin ester is that its mass fraction of 92.46g(is 12.8%), the quality of monoglyceride is that its mass fraction of 1.95g(is 0.27%);
3, ultrasonic wave is auxiliary mixes:
Prepared water phase wall material solution and oil phase core material solution are mixed under the water bath condition of temperature 60 C, the auxiliary 5min that stirs of ultrasonic wave, obtain mixed solution.In mixed solution, the mass ratio of oil phase core material solution and water phase wall material solution is 1:1.4;
4, high-shear emulsifying:
By high-shear emulsion machine, resulting mixed solution is carried out to emulsification, the shearing rotating speed is 10000r/min, and the time is 5min; Obtain emulsion;
5, high-pressure homogeneous:
By resulting emulsion, be under the 25MPa condition at pressure, homogeneous 4 times;
6, spray-drying:
By the spray-drying under the condition of 191 ℃ of EATs, 60 ℃ of feeding temperatures, 7 ml/min charging pump speeds, 400L/h air mass flow of the emulsion after high-pressure homogeneous;
7, screening:
The powder that spray-drying makes is crossed to 100 mesh sieves, get final product to obtain the phytosterin ester microcapsule product.
Prepared phytosterin ester microcapsule product is faint yellow, and big or small homogeneous has micro-sweet fragrant, and embedding rate is 96.45%, and solubility is 97.12%.
Claims (3)
1. the preparation method of phytosterin ester microcapsules is characterized in that:
(1). the preparation of water phase wall material solution:
Get Arabic gum and be dissolved in the temperature 60 C deionized water, add maltodextrin to dissolve, at the temperature 60 C Water Under, bathe standing 30min, then add sucrose ester to mix, make water phase wall material solution; In water phase wall material solution, the mass fraction of Arabic gum is 4.13%～14.37%, and the mass fraction of maltodextrin is 3.44%～12.93%, and the mass fraction of sucrose ester is 0.8%～1.87%;
(2). the preparation of oil phase core material solution:
In phytosterin ester, add monoglyceride, mix, make oil phase core material solution; In oil phase core material solution, the mass fraction of phytosterin ester is 10.33%～21.56%, and the mass fraction of monoglyceride is 0.2%～0.47%;
(3). ultrasonic wave is auxiliary to be mixed:
Water phase wall material solution and oil phase core material solution are mixed under the water bath condition of temperature 60 C, the auxiliary 5min that stirs of ultrasonic wave, obtain mixed solution; In mixed solution, the mass ratio of oil phase core material solution and water phase wall material solution is 1:0.5～1:3;
(4). high-shear emulsifying:
In high-shear emulsion machine, mixed solution is carried out to emulsification, the shearing rotating speed is 10000r/min, and the time is 5min, obtains emulsion;
(5). high-pressure homogeneous:
By emulsion, at pressure, be under 20MPa～40MPa condition with high pressure homogenizer, homogeneous 2～4 times;
(6). spray-drying:
By the spray-drying under the air mass flow condition of the charging pump speed of 175 ℃ of the temperature～EAT of 195 ℃, the feeding temperature of temperature 60 C, 4.5ml/min～7.5ml/min, 350L/h～400L/h of the emulsion after homogeneous;
(7). screening:
The powder that spray-drying makes is crossed to 100 mesh sieves, obtain the phytosterin ester microcapsules, phytosterin ester microcapsule size homogeneous, have micro-sweet fragrant, and embedding rate is greater than 94%, and solubility is greater than 95%.
2. the preparation method of a kind of phytosterin ester microcapsules according to claim 1, it is characterized in that: the percent value that reduced sugar in described maltodextrin (take glucose meter) accounts for the syrup dry is 15～20, and the hydrophilic hydrophobic balance value (HLB) of described sucrose ester is 15.
3. the preparation method of a kind of phytosterin ester microcapsules according to claim 1, it is characterized in that: the hydrophilic hydrophobic balance value (HLB) of described monoglyceride is 3.8, in described phytosterin ester, contain cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester, the total content of cupreol ester, stigmasterol ester, brassicasterol ester and campesterol ester is greater than 98%.
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Application publication date: 20131127 |