CN102485736A - Method of extracting high purity rebaudiodside A from stevioside at normal temperature - Google Patents
Method of extracting high purity rebaudiodside A from stevioside at normal temperature Download PDFInfo
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- CN102485736A CN102485736A CN2010105687680A CN201010568768A CN102485736A CN 102485736 A CN102485736 A CN 102485736A CN 2010105687680 A CN2010105687680 A CN 2010105687680A CN 201010568768 A CN201010568768 A CN 201010568768A CN 102485736 A CN102485736 A CN 102485736A
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Abstract
The invention discloses a method of extracting high purity rebaudiodside A from stevioside at normal temperature. The method comprises the following steps: with stevioside as a raw material, dissolving stevioside with a mixed solvent of methanol and ethanol mixed according to a ratio of 1:0.5 to 1:2.5, standing an obtained mixture for 12 to 48 h at normal temperature, precipitating a crystal, carrying out filtering so as to obtain the crystal, carrying out recrystallization on mother liquor so as to obtain a recrystallized crystal, merging the crystal and the recrystallized crystal, dissolving the merged crystal with a mixed solvent of isopropanol and ethanol mixed according to a ratio of 1:0.5 to 1:3, carrying out ultrasonic extraction for 5 to 20 min at normal temperature, carrying out secondary crystallization, repeating ultrasonic extraction once to three times, carrying out filtering so as to obtain a crystal and subjecting the crystal obtained after filtration to vacuum drying at a temperature of 60 to 80 DEG C so as to eventually obtain a product in which the content of rebaudiodside A is more than or equal to 95%. According to the invention, based on the fact that rebaudiodside A and other glucoside have different solubility in different solvents, rebaudiodside A is separated from other components, and rebaudiodside A in the product has a purity of more than 95% and yield of more than 80%; the method has simple process flow and is suitable for industrial production.
Description
Technical field
The present invention relates to from stevioside, extract under a kind of normal temperature method, the especially dna purity of high purity Lai Baodi glycosides A method greater than the Lai Baodi glycosides A more than 95%.
Background technology
Stevioside is a kind of a kind of pure natural that from the leaf of sweet Stevia, extracts, high sugariness, low heat value, edible safety, is to continue to have outside sucrose, the beet sugar exploitation to be worth and healthy natural sweeteners of praising highly, and is described as " third place in the world sucrose " in the world.Its sugariness is 200～350 times of sucrose, but heat is merely sucrose 1/300.The steviol glycoside acid and alkali-resistance, to Heat stability is good, no fermentable, can keep for a long time in that the solution of PH3～9 is red, also not decomposing, can be widely used among the sugared fields of nearly all usefulness such as video, beverage, wine brewing, medicine, essence and flavoring agent up to 200 ℃.Stevioside low heat value and edible safety; Illnesss such as hypertension, hyperglycemia there is certain adjuvant treatment effect; It is edible to be suitable for specific crowds such as mellitus, hypertension, obesity, also is simultaneously to pursue ideal sucrose substitute healthy, that advocate natural people in modern.
Steviol glycoside is the mixture of a kind of stevia rebaudianum alcohol sugar, mainly contains steviol glycoside (Stevioside), Lai Baodi glycosides A (Rebaudioside A), Lai Baodi glycosides C (Rebaudioside C) but and Dole's glycosides A polysaccharide components such as (Dulcoside A).The sugariness of steviol glycoside is 200 times of sucrose, but it has certain bad pleasant impression.The sugariness of Lai Baodi C glycosides is less than 50 times of sucrose, and stronger back bitter taste and bad pleasant impression are arranged.The sugariness of Lai Baodi glycosides A is 250～450 times of sucrose, and outward appearance is white powder or crystal, and is soluble in water.Best substitute for sucrose; General steviol glycoside purity is 80～95%, and wherein Lai Baodi glycosides A purity is 20～90%, has certain peculiar smell; Be difficult to directly directly use as independent composition; But the high purity Lai Baodi glycosides A that purity reaches more than 95% can directly use as foodstuff additive, can apply in the sugared fields of nearly all usefulness such as the huge beverage of sugared demand, wine brewing, food, medicine.
Therefore, how to improve the content rebaudioside-A product gas purity, develop the Technology of low-cost suitability for industrialized production high purity content rebaudioside-A product, be the focus that each Steviosides manufacturing enterprise and correlative study personnel pay close attention to always.
Have common structural motif stevia rebaudianum alcohol radical between the different stevia rebaudianum alcohol glucosides, structure is very similar each other, separates to get up the comparison difficulty.Through effort and practice for many years, people have have researched and developed out the Technology of various production high purity content rebaudioside-A products and have applied for relevant patent.Overview is got up, and main technology method has HPLC, tlc, chromatography, supercritical extraction, crystallization process etc.Most economical, effective means is a recrystallization method; Utilize different stevia rebaudianums alcohol glucosides dissolubility difference in a certain specific TR in some solvent to carry out crystallization, recrystallization; Realize effective separation and enrichment between the component of different glucosides, thereby obtain highly purified content rebaudioside-A product.Recrystallisation solvent commonly used has lower aliphatic alcohols (like methyl alcohol, ethanol, Virahol, butanols) and other organic solvents (like ETHYLE ACETATE, acetone) etc.In " food and machinery " (26 the 1st phase of volume) " recrystallization method separates the technical study of stevioside " literary composition of the 160th page of publishing in January, 2010; The best crystallization condition and the solvent that have disclosed content rebaudioside-A are selected; Its crystallization processes need carry out crystallization under five degrees below zero condition Celsius; Need large-scale refrigerating apparatus, increased demand facility investment.
Summary of the invention
The objective of the invention is to disclose the method for from stevioside, extracting highly purified Lai Baodi glycosides A under a kind of normal temperature; Utilize Lai Baodi glycosides A and the different solubility of other glucosides in different solvents; Through utilizing in the total glycosides of all kinds of SOLVENTS polarity difference and stevioside difference and the cavitation effect of ultrasonic waves of several kinds of compositions, reach the purpose of Lai Baodi glycosides A and other component separating at opposed polarity dissolution with solvents degree.
The present invention realizes through following technical scheme:
From stevioside, extract the method for highly purified Lai Baodi glycosides A under a kind of normal temperature, realize through following steps:
At first in crystallizer, add blending ratio and be 1: 0.5～1: 2.5 methyl alcohol and alcohol mixed solvent, add weight ratio again and be 1: 5～1: 8 stevioside raw material, stirring and dissolving; Normal temperature held 12～48 hours is separated out crystal, filters to obtain crystal; With mother liquor once more recrystallization once obtain the recrystallization crystal, merge the crystal that obtains for twice; The use blending ratio is 1: 0.5～1: 3 Virahol and alcohol mixed solvent dissolving, and said crystallisate and said Virahol and alcohol mixed solvent weight ratio are 1: 5～1: 8, repeat ultrasonic extraction at normal temperatures 1～3 time; Each extraction 5～20 minutes, and carry out solid-liquid separation, filter and obtain crystal; With the crystal drying under reduced pressure that obtains 5～10 hours, obtain Lai Baodi glycosides A content at last more than or equal to 95% product.
As the further improvement of such scheme, said drying under reduced pressure carries out under 60～80 ℃ of temperature.
Principle of the present invention is: common stevioside is a kind of mixture of stevia rebaudianum alcohol sugar, mainly contains steviol glycoside (Stevioside), Lai Baodi glycosides A (Rebaudios ide A), Lai Baodi glycosides C polysaccharide components such as (Rebaudioside C).Be soluble in methyl alcohol and the ethanol; But the different solubility of different glucosides in different solvents; Steviol glycoside (Stevioside) is soluble in the stronger ethanol of polarity; Lai Baodi glycosides A (Rebaudioside A) is slightly soluble then, and this technology is utilized the difference of the solubleness of several kinds of compositions in the opposed polarity solvent in methyl alcohol and the stevioside general glycoside different with the ethanol polar under the state of normal pressure and temperature; Through the ratio of adjustment different solvents, with the Lai Baodi glycosides A in the stevioside general glycoside and other component separating.Use single mixed solvent to repeat crystallization and further improve Lai Baodi glycosides A content and the very difficult realization of Lai Baodi glycosides A extraction yield; Utilize the different secondary of several kinds of compositional polarities in the stevioside general glycoside to adopt Virahol and ethanol mixed solvent to utilize cavitation effect of ultrasonic waves, make Lai Baodi glycosides A content improve.The inventive method is to utilize the dissolving properties of Lai Baodi glycosides A and other glucosides; Adopt recrystallization method earlier; Utilize methyl alcohol with ethanol mixed solvent Lai Baodi glycosides A to be separated, purifies with other glucosides, the content of the Lay Bao glucosides A that process is purified is in 90% (HPLC detection).Crystallisate after the purification separates once more, purifies with alcohol mixed solvent with Virahol; Use the UW re-extract for several times simultaneously; Utilize the difference of Lai Baodi glycosides A solubleness in different solvents; Simultaneously carry out ultrasonic assisting crystallisation by the ultrasonic cavitation effect, the Lai Baodi glycosides A content that advanced secondary crystal reaches more than 95%.
The inventive method advantage is that product purity is high, productive rate is high, the market cost is low, is fit to suitability for industrialized production.
Description of drawings
Combine embodiment that the present invention is done further description with reference to the accompanying drawings.
Fig. 1 is a FB(flow block) of the present invention,
Fig. 2 is Lai Baodi glycosides A reference substance HPLC numeric distribution figure,
Fig. 3 is crystallisate Lai Baodi glycosides A HPLC numeric distribution figure,
Fig. 4 is refined products Lai Baodi glycosides A HPLC numeric distribution figure.
Embodiment
Embodiment 1
Referring to Fig. 1, take by weighing commercially available stevioside, going out wherein through the HPLC check and analysis, Lai Baodi glycosides A content is 50% (see figure 2).Add in the crystallizer, additional proportion is 1: 2 methyl alcohol-alcohol mixed solvent, is 1: 5 stirring and dissolving by solid-to-liquid ratio, leaves standstill 48 hours; Filter, obtain crystallisate,, filter liquid crystallization once more; Merge crystal twice, utilize performance liquid method detection level result to see Fig. 3, add the Virahol-ethanol mixed solvent of 1: 6 ratio, the use ultrasonic power is 500～2000W; Frequency is the ultrasonic generator ultrasonic extraction 15 minutes of 20～40Khz, filters, and crystal is repeated ultrasonic extraction once; And adopt plate-and-frame filter press or separating centrifuge to carry out solid-liquid separation, and filter and collect crystal grain, carry out drying under reduced pressure then; The drying temperature of drying under reduced pressure is 60～80 ℃, and the time is 5～10 hours, finally obtains finished product.The content that product is carried out HPLC check and analysis Lai Baodi glycosides A is 98.1%, and the result sees Fig. 4.Yield is 83.4%.
Embodiment 2
Take by weighing commercially available stevioside, going out wherein through the HPLC check and analysis, Lai Baodi glycosides A content is 60%.Add in the crystallizer, additional proportion is 1: 2.5 methyl alcohol-alcohol mixed solvent, is 1: 6 stirring and dissolving by solid-to-liquid ratio, leaves standstill 36 hours; Filter, obtain crystallisate,, filter liquid crystallization once more; Merge crystal twice, add the Virahol-ethanol mixed solvent of 1: 5 ratio, ultrasonic 18 minutes; Filter, crystal is repeated ultrasonic extraction once, and carry out solid-liquid separation and filter the collection crystal grain.Carry out drying under reduced pressure then, get product, the content that product is carried out HPLC check and analysis Lai Baodi glycosides A is 97.9%, and yield is 82.9%.
Embodiment 3
Take by weighing commercially available stevioside, going out wherein through the HPLC check and analysis, Lai Baodi glycosides A content is 40%.Add in the crystallizer, additional proportion is 1: 1.5 methyl alcohol-alcohol mixed solvent, is 1: 8 stirring and dissolving by solid-to-liquid ratio, leaves standstill 48 hours; Filter, obtain crystallisate,, filter liquid crystallization once more; Merge crystal twice, add the Virahol-ethanol mixed solvent of 1: 5 ratio, ultrasonic 10 minutes; Filter, crystal is repeated ultrasonic extraction once, and carry out solid-liquid separation and filter the collection crystal grain.Carry out drying under reduced pressure then, get product, the content that product is carried out HPLC check and analysis Lai Baodi glycosides A is 98.6%, and yield is 83.2%.
Above-mentionedly the technology of the Lai Baodi glycosides A of separating high-purity is described in detail with reference to instance; Be illustrative rather than determinate; For those of ordinary skill in the art; Be appreciated that under the situation that does not break away from principle of the present invention and spirit and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited accompanying claims and equivalent thereof.
Claims (4)
1. from stevioside, extract the method for highly purified Lai Baodi glycosides A under the normal temperature, it is characterized in that: at first in crystallizer, add blending ratio and be 1: 0.5～1: 2.5 methyl alcohol and alcohol mixed solvent, add the weight ratio ratio again and be 1: 5～1: 8 stevioside raw material; Stirring and dissolving, normal temperature held 12～48 hours is separated out crystal; Filtration obtains crystal, with mother liquor once more recrystallization once obtain the recrystallization crystal; Merge the crystal that obtains for twice, using blending ratio is that 1: 0.5～1: 3 Virahol dissolves with alcohol mixed solvent, and said crystallisate and said Virahol and alcohol mixed solvent weight ratio are 1: 5～1: 8; Repeat ultrasonic extraction at normal temperatures and carry out secondary crystal 1～3 time; Each extraction 5～20 minutes, and carry out solid-liquid separation, filter and obtain crystal; With the crystal drying under reduced pressure that obtains 5～10 hours, obtain Lai Baodi glycosides A content at last more than or equal to 95% product.
2. according to the method for from stevioside, extracting highly purified Lai Baodi glycosides A under the described a kind of normal temperature of claim 1, it is characterized in that: said drying under reduced pressure carries out under 60～80 ℃ of temperature.
3. according to the method for from stevioside, extracting highly purified Lai Baodi glycosides A under the described a kind of normal temperature of claim 1; It is characterized in that: what said ultrasonic extraction was adopted is that ultrasonic power is 500～2000W, and frequency is that the ultrasonic generator of 20～40Khz extracts.
4. according to the method for from stevioside, extracting highly purified Lai Baodi glycosides A under the described a kind of normal temperature of claim 1, it is characterized in that: said solid-liquid separation adopts plate-and-frame filter press or separating centrifuge to carry out.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013088246A3 (en) * | 2011-12-16 | 2013-11-21 | Almendra Pte Ltd. | Process for the purification of rebaudioside a and compositions thereof |
| CN104098739A (en) * | 2013-04-09 | 2014-10-15 | 江南大学 | Preparation method for rebaudiodside A molecularly-imprinted polymer |
| CN110150625A (en) * | 2019-07-03 | 2019-08-23 | 史迪威生物科技（苏州）有限公司 | A kind of glycoside composition, edible composition and beverage |
| CN111662344A (en) * | 2020-06-29 | 2020-09-15 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
| CN113461746A (en) * | 2021-08-11 | 2021-10-01 | 郑然� | Refining method of high-purity stevioside RA |
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| US4361697A (en) * | 1981-05-21 | 1982-11-30 | F. K. Suzuki International, Inc. | Extraction, separation and recovery of diterpene glycosides from Stevia rebaudiana plants |
| US5962678A (en) * | 1996-09-13 | 1999-10-05 | Alberta Research Council | Method of extracting selected sweet glycosides from the Stevia rebaudiana plant |
| CN101591366A (en) * | 2009-07-07 | 2009-12-02 | 天津美伦医药集团有限公司 | The technology of 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 |
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2010
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| US5962678A (en) * | 1996-09-13 | 1999-10-05 | Alberta Research Council | Method of extracting selected sweet glycosides from the Stevia rebaudiana plant |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013088246A3 (en) * | 2011-12-16 | 2013-11-21 | Almendra Pte Ltd. | Process for the purification of rebaudioside a and compositions thereof |
| 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 |
| CN110150625A (en) * | 2019-07-03 | 2019-08-23 | 史迪威生物科技（苏州）有限公司 | A kind of glycoside composition, edible composition and beverage |
| CN111662344A (en) * | 2020-06-29 | 2020-09-15 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
| CN111662344B (en) * | 2020-06-29 | 2022-10-14 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
| CN113461746A (en) * | 2021-08-11 | 2021-10-01 | 郑然� | Refining method of high-purity stevioside RA |
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Application publication date: 20120606 |