CN101240224A - Method for preparing sweet orange essence microcapsule - Google Patents
Method for preparing sweet orange essence microcapsule Download PDFInfo
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- CN101240224A CN101240224A CNA2008100707125A CN200810070712A CN101240224A CN 101240224 A CN101240224 A CN 101240224A CN A2008100707125 A CNA2008100707125 A CN A2008100707125A CN 200810070712 A CN200810070712 A CN 200810070712A CN 101240224 A CN101240224 A CN 101240224A
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- aqueous solution
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Abstract
A preparation method for sweet orange essence microcapsule relates to a preparation technology of essence microcapsule. A preparation method for sweet orange essence microcapsule is provided with simple technology, safe and controlled operation, collapse and excellent releasing performance microcapsule wall film. The preparation steps comprise bean separation albumen aqueous solution and Arabic gum aqueous solution is prepared, an emulsion is obtainer by putting sweet orange essence into bean separation albumen aqueous solution and homogenizing, a wet microcapsule is obtained by putting and mixing Arabic gum aqueous solution into emulsion and putting alcaine or acetic acid to adjust PH to 4.0. The reinforced wet microcapsule is obtained by cooling the wet microcapsule down to 0 to 15 DEG C and dextrose being putting into the solution concomitant mixing. The powder-shaped sweet orange essence microcapsule can be obtained by putting the reinforced wet microcapsule into ultra low temperature ice box and drying the reinforced wet microcapsule in vacuum freeze drier.
Description
Technical field
The present invention relates to a kind of preparation technology of essence microcapsule, the variation that especially relates to a kind of pH of utilization value comes the complex coacervation system of regulating and controlling soybean protein isolate (SPI) and gum arabic to prepare the technology of microcapsule.
Background technology
The essence microcapsule technology is that finely dispersed xiang semen is dripped off total incapsulation forms microcapsule in a skim a kind of technology; essence is behind micro encapsulation; the sealing function of cyst wall can effectively suppress the volatilization loss of essence; protect responsive composition; not only improve the oxytolerant of essence, fast light and heat-stable ability greatly, also improved the storage of essence and the stability of use effectively.
The common method of micro encapsulation has reached kind more than 200 at present, yet these methods respectively have relative merits, consider the specific properties of essence, and the suitable technology of preparing that can reach its requirement is seldom arranged.Wherein emulsification is spray-dired is most widely used, and accounts for 90% of existing market, but the capsule embedding rate of this method preparation is not high and the rate of recovery is low, and high temperature drying makes the part component volatilization of essence or destroyed, thereby causes the odor type distortion of product, mouthfeel clumsiness.The complex coacervation rule is a kind of technology of heat of research recently, is mainly used to embedding volatile oil, is a kind of very promising special microencapsulation technology, and this technical matters is simple, and operational safety is easy to control, the wall film densification of formation, and release performance is good.
Gelatin/gum arabic system is present most widely used complex coacervation system.But gelatin thickness very just when concentration is very low, not only increased operation easier, limited the system solid concentration, and because gelatin is preparation from animal body, some proteolytic enzyme communicate illness may take place in addition, add that the normal linking agent glutaraldehyde that adopts of this system has certain toxicity to human body, this all multifactor its application in industrial production that greatly influenced.Soybean protein isolate then is a kind of functional plants albumen of health, to gelatin very similar iso-electric point is arranged, and is a kind of amphipathic molecule, and its wide material sources are cheap, is that a kind of good microcapsule prepare raw material.And present soybean protein isolate or its hydrolyzate are applied in the spraying drying mostly, and the research that utilizes soybean protein isolate SPI to replace gelatin and gum arabic to carry out the complex coacervation reaction yet there are no report.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, and operational safety is easy to control, the preparation method of the orange flavor microcapsule that the microcapsule wall film densification of formation and release performance are good.
Step of the present invention is as follows:
1) water preparation mass percent concentration is 5%～15% the soybean protein isolate aqueous solution, and is after the ultrasonic pretreatment, standby; Water preparation mass percent concentration is 5%～15% the gum arabic aqueous solution, and is standby;
2) get emulsion behind the adding orange flavor homogeneous in the soybean protein isolate aqueous solution, by mass percentage, the add-on of orange flavor accounts for 10%～20% of soybean protein isolate amount;
3) add the standby gum arabic aqueous solution in the step 1 in emulsion, stir, add hydrochloric acid or acetic acid regulator solution pH to 4.0, reaction obtains wet microcapsule;
4) the wet microcapsule that step 3 is obtained are cooled to 0～15 ℃, add glucose, press mass ratio, soybean protein isolate: the glucose of glucose=10: 1 continues stirring, the wet microcapsule after obtaining reinforcing.
5) the wet microcapsule after the reinforcing that step 4 is obtained place Ultralow Temperature Freezer, promptly obtain pulverous orange flavor microcapsule after placing the vacuum freeze drier drying again.
In step 1), the temperature of water is preferably 50～75 ℃, described water preferably adopts deionized water, and described ultrasonic pretreatment is preferably with the soybean protein isolate aqueous solution supersound process 10min under 600W power that configures, and the protein content of described soybean protein isolate is best＞and 90%.
In step 2) in, the speed that adds orange flavor is preferably 1/s, and the homogeneous rotating speed is 6000r/min, homogenizing time 5min.The temperature of whipping process is preferably 50 ℃.
In step 3), the gum arabic of adding and the mass ratio of soybean protein isolate are 1: 1.The concentration of hydrochloric acid is preferably 10%, and the adding speed of HCl is preferably 1/10s, can effectively prevent capsular cohering, and the time of stirring is best＞30min, the rotating speed of stirring is preferably 1300r/min.The concentration of acetic acid is preferably 10%, and adding speed is not cohered with capsule and is advisable.
In step 4), the ice bath cooling is preferably adopted in described cooling, and the time of stirring is preferably 1～2h, and the rotating speed of stirring is preferably 850r/min.Can add micro-pectin when adding glucose, the add-on of pectin is 2%～5% of a glucose quality.The time that continues to stir is preferably 1～2h.
In step 5), Ultralow Temperature Freezer preferably adopts-80 ℃.
Compared with the prior art, the present invention has following outstanding advantage and effect:
Because the present invention adopts the wall material of soybean protein isolate as microcapsule, therefore overcome the defective that gelatin gum arabic complex coacervation system exists, reduced production cost, and in conjunction with complex coacervation reactive system and Vacuum Freezing ﹠ Drying Technology, go out uniform particles, cyst wall densification, the essence microcapsule that release performance is good by simple prepared.The present invention is particularly suitable for highly volatile or rotten liquid ingredient are prepared into the pressed powder of easy storage and transport.
Description of drawings
Fig. 1 is the Electronic Speculum figure of the orange flavor microcapsule of the embodiment of the invention 1 gained.
Embodiment
The present invention is further illustrated by following examples and accompanying drawing.
Embodiment 1
Concrete processing step:
1. the preparation of microcapsule wall material solution and processing
Get the soybean protein isolate spi protein 100g of protein content＞90%, with adopting the 600W ultrasonic apparatus behind the deionized water dissolving of 50 ℃ of 900g, ultrasonic 10min obtains concentration and be 10% the soybean protein isolate spi protein aqueous solution, and is standby; Get gumwater 100g, after the abundant stirring and dissolving of deionized water with 50 ℃ of 900g, concentration is 10% the gum arabic aqueous solution, standby;
2. emulsification homogeneous
Dropwise 5 mL orange flavor in the standby soybean protein isolate SPI solution in step 1,50 ℃ of water-baths, homogeneous (using 6000r/min) 5min, emulsion;
3, complex coacervation
In the emulsion of step 2 gained, add standby gumwater in the step 1, drip the HCl of concentration 10% after stirring with the speed of 1/10s, regulate pH to 4.0, continue to stir, rotating speed maintains 1300r/min, reacts 30min;
4, the solution ice bath with step 3 gained is cooled to below the room temperature, adds glucose 1g and the crosslinked 2h of pectin 0.02g again, continues to stir, and rotating speed maintains 850r/min, the wet microcapsule after obtaining reinforcing;
5, place Ultralow Temperature Freezer (80 ℃) to spend the night the wet microcapsule of step 4 gained after, can collect the sweet orange microcapsule shaping powder-product that obtains after placing the vacuum freeze drier drying.
Fig. 1 has provided the exterior appearance that adopts the observed microcapsule product of scanning electron microscope sem.As seen from Figure 1, capsule particle is even, and particle diameter is at 5～10 μ m, outward appearance slyness, the densification of wall film; The embedding rate that adopts volatile oil determination apparatus to measure the capsule product that obtains is 62.73%, and product is perfume ingredient loss＜20% behind 105 ℃ of high bake 10h; The component that adopts GC-MS to detect the essence embedding front and back does not have to change substantially.Through check, the microcapsule product color and luster that obtains is yellowish, and fragrance is joyful, and flowability and dispersiveness are all better.
Embodiment 2
Similar to Example 1, difference is: the soybean protein isolate SPI in the step 1 and gum arabic are formulated as the aqueous solution of 15% concentration respectively, and the orange flavor addition is 7.5mL.
After testing, the embedding rate that adopts volatile oil determination apparatus to measure the capsule product that obtains is 69.52%, and product is perfume ingredient loss＜20% behind 105 ℃ of high bake 10h; The component that adopts GC-MS to detect the essence embedding front and back does not have to change substantially.
Embodiment 3
Similar to Example 1, difference is: the soybean protein isolate SPI in the step 1 and gum arabic are formulated as the aqueous solution of 5% concentration respectively, and the orange flavor addition is 2.5mL.
After testing, the embedding rate that adopts volatile oil determination apparatus to measure the capsule product that obtains is 59.84%, and product is perfume ingredient loss＜20% behind 105 ℃ of high bake 10h; The component that adopts GC-MS to detect the essence embedding front and back does not have to change substantially.
Embodiment 4
Similar to Example 1, difference is: with the orange flavor addition in the step 2 is 2.5mL.
After testing, the embedding rate that adopts volatile oil determination apparatus to measure the capsule product that obtains is 89.52%, and product is perfume ingredient loss＜20% behind 105 ℃ of high bake 10h; The component that adopts GC-MS to detect the essence embedding front and back does not have to change substantially.
Embodiment 5
Similar to Example 1, difference is: with the orange flavor addition in the step 2 is 3.5mL.
After testing, the embedding rate that adopts volatile oil determination apparatus to measure the capsule product that obtains is 79.12%, and product is perfume ingredient loss＜20% behind 105 ℃ of high bake 10h; The component that adopts GC-MS to detect the essence embedding front and back does not have to change substantially.
Claims (10)
1. the preparation method of orange flavor microcapsule is characterized in that its step is as follows:
1) water preparation mass percent concentration is 5%～15% the soybean protein isolate aqueous solution, and is after the ultrasonic pretreatment, standby; Water preparation mass percent concentration is 5%～15% the gum arabic aqueous solution, and is standby;
2) get emulsion behind the adding orange flavor homogeneous in the soybean protein isolate aqueous solution, by mass percentage, the add-on of orange flavor accounts for 10%～20% of soybean protein isolate amount;
3) add the standby gum arabic aqueous solution in the step 1 in emulsion, stir, add hydrochloric acid or acetic acid regulator solution pH to 4.0, reaction obtains wet microcapsule;
4) the wet microcapsule that step 3 is obtained are cooled to 0～15 ℃, add glucose, press mass ratio, soybean protein isolate: the glucose of glucose=10: 1 continues stirring, the wet microcapsule after obtaining reinforcing.
5) the wet microcapsule after the reinforcing that step 4 is obtained place Ultralow Temperature Freezer, promptly obtain pulverous orange flavor microcapsule after placing the vacuum freeze drier drying again.
2. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 1), and the temperature of water is 50～75 ℃.
3. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 1), and described ultrasonic pretreatment is the soybean protein isolate aqueous solution supersound process 10min under 600W power that will configure.
4. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 1), the protein content of described soybean protein isolate＞90%.
5. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 2) in, the speed that adds orange flavor is 1/s, the homogeneous rotating speed is 6000r/min, homogenizing time 5min; The temperature of whipping process is 50 ℃.
6. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 3), and the gum arabic of adding and the mass ratio of soybean protein isolate are 1: 1.
7. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 3), and the concentration of hydrochloric acid is 10%, and the adding speed of hydrochloric acid is 1/10s, and the time＞30min of stirring, the rotating speed of stirring are 1300r/min.
8. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 3), and the concentration of acetic acid is 10%.
9. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 4), and the described ice bath that is cooled to cools off, and the time of stirring is 1～2h, and the rotating speed of stirring is 850r/min.
10. the preparation method of a kind of orange flavor microcapsule as claimed in claim 1 is characterized in that in step 4), adds micro-pectin when adding glucose, and the add-on of pectin is 2%～5% of a glucose quality; The time that continues to stir is 1～2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100707125A CN101240224B (en) | 2008-03-07 | 2008-03-07 | Method for preparing sweet orange essence microcapsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100707125A CN101240224B (en) | 2008-03-07 | 2008-03-07 | Method for preparing sweet orange essence microcapsule |
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| Publication Number | Publication Date |
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| CN101240224A true CN101240224A (en) | 2008-08-13 |
| CN101240224B CN101240224B (en) | 2010-08-25 |
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| CN2008100707125A Expired - Fee Related CN101240224B (en) | 2008-03-07 | 2008-03-07 | Method for preparing sweet orange essence microcapsule |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190805A (en) * | 2010-03-05 | 2011-09-21 | 吉林农业大学 | Method for raising mechanical strength of soybean protein edible films by using ultrasonic treatment |
| CN101708451B (en) * | 2009-12-25 | 2011-11-09 | 陕西科技大学 | Method for preparing high-temperature resistant essence microcapsules |
| CN103451019A (en) * | 2013-09-04 | 2013-12-18 | 湖北中烟工业有限责任公司 | Microcapsule essence perfume for cigarettes as well as preparation method of microcapsule essence perfume |
| CN105054074A (en) * | 2015-07-01 | 2015-11-18 | 浙江海洋学院 | Surimi enzymatic hydrolysis peptide chelated iron (II) anti-oxidation microcapsule and preparation technology thereof |
| CN106245342A (en) * | 2016-07-28 | 2016-12-21 | 江苏汉诺斯化学品有限公司 | A kind of be wall material with blackberry extract microcapsule and preparation method thereof |
| CN108782924A (en) * | 2018-05-11 | 2018-11-13 | 中玺（天津）枣业技术工程中心 | Jujube maltose and preparation method thereof |
| CN110367538A (en) * | 2019-08-23 | 2019-10-25 | 齐鲁工业大学 | A method of agglomerating preparation essential oil microcapsules again using soybean protein/carboxymethyl starch |
| CN111418889A (en) * | 2020-03-16 | 2020-07-17 | 云南中烟工业有限责任公司 | Neroli oil capsule dry bead, preparation method thereof and application thereof in tobacco |
| WO2021072505A1 (en) * | 2019-10-16 | 2021-04-22 | Clover Corporation Limited | Protein encapsulation of nutritional and pharmaceutical compositions |
| CN114376972A (en) * | 2021-12-30 | 2022-04-22 | 浙江工商大学 | Eugenol emulsion with slow transdermal function and stabilized by SPI-GA conjugate and compound and application |
| WO2023232432A1 (en) * | 2022-05-31 | 2023-12-07 | Unilever Ip Holdings B.V. | Microcapsule and method |
-
2008
- 2008-03-07 CN CN2008100707125A patent/CN101240224B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708451B (en) * | 2009-12-25 | 2011-11-09 | 陕西科技大学 | Method for preparing high-temperature resistant essence microcapsules |
| CN102190805A (en) * | 2010-03-05 | 2011-09-21 | 吉林农业大学 | Method for raising mechanical strength of soybean protein edible films by using ultrasonic treatment |
| CN103451019A (en) * | 2013-09-04 | 2013-12-18 | 湖北中烟工业有限责任公司 | Microcapsule essence perfume for cigarettes as well as preparation method of microcapsule essence perfume |
| CN105054074A (en) * | 2015-07-01 | 2015-11-18 | 浙江海洋学院 | Surimi enzymatic hydrolysis peptide chelated iron (II) anti-oxidation microcapsule and preparation technology thereof |
| CN106245342A (en) * | 2016-07-28 | 2016-12-21 | 江苏汉诺斯化学品有限公司 | A kind of be wall material with blackberry extract microcapsule and preparation method thereof |
| CN108782924A (en) * | 2018-05-11 | 2018-11-13 | 中玺（天津）枣业技术工程中心 | Jujube maltose and preparation method thereof |
| CN110367538A (en) * | 2019-08-23 | 2019-10-25 | 齐鲁工业大学 | A method of agglomerating preparation essential oil microcapsules again using soybean protein/carboxymethyl starch |
| WO2021072505A1 (en) * | 2019-10-16 | 2021-04-22 | Clover Corporation Limited | Protein encapsulation of nutritional and pharmaceutical compositions |
| CN114786505A (en) * | 2019-10-16 | 2022-07-22 | 科劳弗股份有限公司 | Protein encapsulation of nutritional and pharmaceutical compositions |
| CN111418889A (en) * | 2020-03-16 | 2020-07-17 | 云南中烟工业有限责任公司 | Neroli oil capsule dry bead, preparation method thereof and application thereof in tobacco |
| CN114376972A (en) * | 2021-12-30 | 2022-04-22 | 浙江工商大学 | Eugenol emulsion with slow transdermal function and stabilized by SPI-GA conjugate and compound and application |
| WO2023232432A1 (en) * | 2022-05-31 | 2023-12-07 | Unilever Ip Holdings B.V. | Microcapsule and method |
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| CN101240224B (en) | 2010-08-25 |
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