CN101100477A - Method for extracting high pure rebaudioside A from stevia sugar - Google Patents
Method for extracting high pure rebaudioside A from stevia sugar Download PDFInfo
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- CN101100477A CN101100477A CNA2007100257928A CN200710025792A CN101100477A CN 101100477 A CN101100477 A CN 101100477A CN A2007100257928 A CNA2007100257928 A CN A2007100257928A CN 200710025792 A CN200710025792 A CN 200710025792A CN 101100477 A CN101100477 A CN 101100477A
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Abstract
A method for extracting high-purity laibaody A glycoside from sweet synanthrin is carried out by taking sweet synanthrin containing laibaody A glycoside 30% as raw material, dissolving sweet synanthrin by mixed solvent of methanol and isopropyl alcohol, crystallizing at -18 deg. C for 24-48 hrs, crystallizing at 4 deg. C for 24-48 hrs, filtering to obtain crystal, re-crystallizing to obtain re-crystallizing crystal, dissolving by pure water 10-20L, separating by film with trapping molecular weight 500, concentrating, and drying below 70 deg. C at 0.08 MPa vacuum for 12-24 hrs to obtain final product. The water content is 3.48%, gray content is 0.26%, laibody A glycoside content is more than 90%, and sweet flavor is as 300 times as cane sugar. It tastes pure.
Description
Technical field
A kind of method of extracting high pure rebaudioside A from stevioside belongs to technical field of food additives.The present invention relates to the production method of efficiency natural sweeting agent in a kind of foodstuff additive field, refer in particular to a kind of from stevioside dna purity greater than the method for 90% rebaudioside A.
Background technology
Stevioside is the natural sweeteners that extracts from the leaf of sweet Stevia.It has the characteristics of high sugariness, low heat energy, is to continue to have exploitation to be worth and healthy natural sweeteners of praising highly outside sucrose, the beet sugar, is described as " third place in the world sucrose " in the world.China is the major country of production of stevioside in the world, produces 700～800 tons per year.Stevioside can be used as sucrose substitute, replaces some artificial synthetic sweeting agent such as Sodium Cyclamate, asccharin etc., is widely used in industries such as food, beverage, and with compare escapable cost 70% with sucrose.
Stevioside is a polycomponent glucoside mixture, and sugariness and mouthfeel depend on its glucoside composition and content.In the known 9 kinds of glucosides of stevioside, higher (stevioside is about 50% with stevioside, rebaudioside A and the Lai Baodi C glucoside relative content in total glucoside, rebaudioside A is about 30%, and Lai Baodi C glucoside is about 10%), also be the main component that influences taste of ribaudiose.The molecular structure of the main glucoside of stevioside:
Stevioside content rebaudioside-A vegetable baudy glucoside C
The sugariness of stevioside is 200 times of sucrose, but it has certain bad pleasant impression.The sugariness of Lai Baodi C glucoside is less than 50 times of sucrose, and stronger back bitter taste and bad pleasant impression are arranged.The sugariness of rebaudioside A is greater than 300 times of sucrose, and flavor matter is also best, does not contain any bad pleasant impression, is a kind of ideal natural sweeteners product.From stevioside (rebaudioside A content is about 30%), extract and purifying high-purity rebaudioside A product, can obtain the pure high sugariness natural sweeteners of mouthfeel.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of and extract efficiency natural sweeting agent--the industrial purifying process of high pure rebaudioside A from stevioside, obtain purity greater than 90% rebaudioside A product.
Technical scheme of the present invention: stevioside is the mixture of multiple glucoside, by the following recrystallization binding film separating technology of process, can obtain purity greater than 90% rebaudioside A product: with methyl alcohol and Virahol (99+1) the mixed solvent dissolving 1kg raw material stevioside (glucoside mixture, wherein rebaudioside A content is about 30%) of 5-8L; Place crystallization 24-48h, continuation placement crystallization 24-48h during the back moves into 4 ℃ prior to-18 ℃; Filtration obtains crystal; With described condition recrystallization once, obtain the recrystallization crystal; The recrystallization crystal is with the dissolving of the pure water of 10-20L, is that 500 membrane sepn is concentrated with molecular weight cut-off; In 70 ℃ of dry 12-24h of 0.08MPa vacuum, obtain the high pure rebaudioside A product.
The invention has the beneficial effects as follows: the natural sweeteners that the inventive method is purified from stevioside--high pure rebaudioside A adopts methyl alcohol and Virahol (99+1) mixing solutions recrystallization method, can remove stevioside and Lai Baodi C glucoside, improve the purity of rebaudioside A greatly; Adopting molecular weight cut-off is that 500 membrane separation technique can be removed ash content, further improves the purity of rebaudioside A, removes dissolvent residual in conjunction with vacuum-drying simultaneously, and the rebaudioside A product moisture content of purification is 3.48%, and ash oontent is 0.26%; Through efficient liquid phase chromatographic analysis, rebaudioside A content is greater than 90%; Sugariness is equivalent to more than 300 times of sucrose, and sweet taste is pure.With common stevioside ratio, mouthfeel is pure, does not have pleasant impression, and sugariness is higher, edible safety.
Description of drawings
The liquid chromatogram of Fig. 1 rebaudioside A standard substance (a) and this handicraft product (b).
Embodiment
Lift several examples below and describe, but be not limited.
Get methyl alcohol and Virahol (99+1) the mixing solutions dissolving 1kg raw material stevioside (glucoside mixture) of 5L; Place crystallization 24h, continuation placement crystallization 48h during the back moves into 4 ℃ prior to-18 ℃; Filtration obtains the about 0.5kg of crystal; With the aforementioned condition recrystallization once, obtain the about 0.25kg of recrystallization crystal; Crystal is with the dissolving of the pure water of 20L, is that 500 membrane sepn is concentrated with molecular weight cut-off; In 0.08MPa vacuum dry 24h below 70 ℃, obtain the about 0.2kg of high pure rebaudioside A product.
The liquid chromatogram of rebaudioside A standard substance (a) and this handicraft product (b) as shown in Figure 1.
High-efficient liquid phase chromatogram condition:
Agilent 100 high performance liquid chromatographs; The 210nm UV-detector;
Chromatographic column: Zorbaxsb C18 post (4.6 * 150mm); Column temperature: 30 ℃;
Moving phase: acetonitrile-water (28+72); Flow velocity: 1mL/min;
Sample size: 10 μ L.
Embodiment 2
Get methyl alcohol and Virahol (99+1) the mixing solutions dissolving 1kg raw material stevioside (glucoside mixture) of 6L; Place crystallization 48h, continuation placement crystallization 24h during the back moves into 4 ℃ prior to-18 ℃; Filtration obtains the about 0.5kg of crystal; With the aforementioned condition recrystallization once, obtain the about 0.25kg of recrystallization crystal; Crystal is with the dissolving of the pure water of 15L, is that 500 membrane sepn is concentrated with molecular weight cut-off; In 0.08MPa vacuum dry 16h below 70 ℃, obtain high pure rebaudioside A product 0.2kg.
Embodiment 3
Get methyl alcohol and Virahol (99+1) the mixing solutions dissolving 1kg raw material stevioside (glucoside mixture) of 8L; Place crystallization 48h, continuation placement crystallization 48h during the back moves into 4 ℃ prior to-18 ℃; Filtration obtains the about 0.5kg of crystal; With the aforementioned condition recrystallization once, obtain the about 0.25kg of recrystallization crystal; Crystal is with the dissolving of the pure water of 10L, is that 500 membrane sepn is concentrated with molecular weight cut-off; In 0.08MPa vacuum dry 12h below 70 ℃, obtain the about 0.2kg of high pure rebaudioside A product.
Claims (2)
1, a kind of method of from stevioside, extracting rebaudioside A, it is characterized in that with the stevioside being raw material, rebaudioside A content is 30% in the control raw material, utilize recrystallization and membrane separation technique to combine, carry out recrystallization with methyl alcohol and 99: 1 methyl alcohol of Virahol volume ratio and isopropyl alcohol mixed solvent 5-8L dissolving 1kg raw material stevioside, place crystallization 24-48h, continuation placement crystallization 24-48h during the back moves into 4 ℃ prior to-18 ℃; Filtration obtains crystal 0.5kg; With described condition again recrystallization once obtain recrystallization crystal 0.25kg; The recrystallization crystal is with the dissolving of the pure water of 10-20L, is 500 membrane sepn with molecular weight cut-off, and is concentrated; In 0.08MPa vacuum dry 12-24h below 70 ℃, obtain high pure rebaudioside A product 0.2kg.
2, the method for extraction rebaudioside A according to claim 1 is characterized in that: the purity of rebaudioside A product is greater than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100257928A CN100500685C (en) | 2007-08-01 | 2007-08-01 | Method for extracting high pure rebaudioside A from stevia sugar |
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| CNB2007100257928A CN100500685C (en) | 2007-08-01 | 2007-08-01 | Method for extracting high pure rebaudioside A from stevia sugar |
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| CN101100477A true CN101100477A (en) | 2008-01-09 |
| CN100500685C CN100500685C (en) | 2009-06-17 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812096A (en) * | 2010-04-21 | 2010-08-25 | 赣州菊隆高科技实业有限公司 | Method for ultrasonically crystallizing rebaudiosideA |
| CN101591366B (en) * | 2009-07-07 | 2012-05-30 | 天津美伦医药集团有限公司 | Process for separating high-purity rebaudioside A |
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
| CN104098739A (en) * | 2013-04-09 | 2014-10-15 | 江南大学 | Preparation method for rebaudiodside A molecularly-imprinted polymer |
| WO2015113370A1 (en) * | 2014-01-30 | 2015-08-06 | 诸城市浩天药业有限公司 | Stevioside a glycoside crystal, preparation method therefor, and uses thereof |
| CN104049047B (en) * | 2014-06-25 | 2015-09-02 | 曲阜圣香远生物科技有限公司 | A kind of method evaluating quality of stevioside |
| CN109563117A (en) * | 2016-08-09 | 2019-04-02 | 帝斯曼知识产权资产管理有限公司 | The crystallization of steviol glycoside |
| CN109651453A (en) * | 2018-12-04 | 2019-04-19 | 江南大学 | A kind of method of high-valued stevioside mother liquor sugar |
-
2007
- 2007-08-01 CN CNB2007100257928A patent/CN100500685C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591366B (en) * | 2009-07-07 | 2012-05-30 | 天津美伦医药集团有限公司 | Process for separating high-purity rebaudioside A |
| CN101812096A (en) * | 2010-04-21 | 2010-08-25 | 赣州菊隆高科技实业有限公司 | Method for ultrasonically crystallizing rebaudiosideA |
| CN104098739A (en) * | 2013-04-09 | 2014-10-15 | 江南大学 | Preparation method for rebaudiodside A molecularly-imprinted polymer |
| CN104098739B (en) * | 2013-04-09 | 2016-05-18 | 江南大学 | The preparation method of rebaudioside A molecularly imprinted polymer |
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
| WO2015113370A1 (en) * | 2014-01-30 | 2015-08-06 | 诸城市浩天药业有限公司 | Stevioside a glycoside crystal, preparation method therefor, and uses thereof |
| CN104049047B (en) * | 2014-06-25 | 2015-09-02 | 曲阜圣香远生物科技有限公司 | A kind of method evaluating quality of stevioside |
| CN109563117A (en) * | 2016-08-09 | 2019-04-02 | 帝斯曼知识产权资产管理有限公司 | The crystallization of steviol glycoside |
| CN109651453A (en) * | 2018-12-04 | 2019-04-19 | 江南大学 | A kind of method of high-valued stevioside mother liquor sugar |
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| Publication number | Publication date |
|---|---|
| CN100500685C (en) | 2009-06-17 |
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