CN102199178A - Extraction process of rebaudioside A (RA) - Google Patents
Extraction process of rebaudioside A (RA) Download PDFInfo
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- CN102199178A CN102199178A CN2011100882978A CN201110088297A CN102199178A CN 102199178 A CN102199178 A CN 102199178A CN 2011100882978 A CN2011100882978 A CN 2011100882978A CN 201110088297 A CN201110088297 A CN 201110088297A CN 102199178 A CN102199178 A CN 102199178A
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Abstract
The invention provides an extraction process for extracting high-purity rebaudioside A (RA) at high efficiency, which comprises the following steps: 1. pulverizing stevia leaves; 2. extracting water-soluble glycoside from the stevia leaves through a subcritical water extraction technique; 3. filtering out impurities from the extracted water-soluble glycoside through a membrane separation technique, and concentrating; 4. carrying out macroporous resin adsorption; and 5. recrystallizing for separation and purification to obtain rebaudioside A (RA). The extraction process provided by the invention increases the extraction speed of stevioside substances and the dissolution rate of stevioside through the subcritical water extraction technique, improves the extraction rate of total glycosides in the raw material to 98% or above, increases the yield of stevioside, quickly extracts the water-soluble glycoside from the stevia leaves, filters out impurities through the membrane separation technique, substitutes for the traditional flocculation process, lowers the production cost, realizes clean production, and uses the macroporous adsorptive resin and recrystallization technique for further separation and purification to obtain the rebaudioside of which the purity is above 90%.
Description
Technical field
The present invention relates to the extraction process of Lai Baodi glucosides RA.
Background technology
Sweet Stevia (
Stevia rebaudiana) have another name called stevia rebaudianum, sugar grass, belong to composite family (
Compositae), the Si Taiwei subgenus originates in South America.The sweet taste substance that extracts from sweet Stevia is called steviol glycoside.Contain 10% the steviol glycoside of having an appointment in the sweet Stevia leaf, wherein Stevioside accounts for 60%～70% of total steviol glycoside, and its sugariness is 300 times of 10% sucrose; Next is Lai Baodi glucosides Rebaudioside A (RA), accounts for 15%～20% of total steviol glycoside, and its sugariness is 450 times of 10% sucrose, and sweet taste is near sucrose.The heat of steviol glycoside is 1/300 of a sucrose only, is a kind of high sugariness, natural health-care low in calories sugar source, and long-term ediblely have health protection and therapeutic action to diseases such as obesity, hypertension, hyperglycemia.
The edible existing centuries history of the resident in steviol glycoside country of origin (ground such as South America Paraguay, Brazil) finds no any murder by poisoning so far.Steviol glycoside is not participated in metabolism in vivo, do not accumulate, and free of toxic effects, its security has obtained the approval of tissues such as international FAO and WHO.Federation of japanese food additive group determines that already steviol glycoside is not for needing the special sweeting agent of limiting the quantity of and using.China Ministry of Health ratified natural sweeteners and the pharmaceutical sweeting agent auxiliary material that steviol glycoside is quantity-unlimiting use in 1985 respectively with nineteen ninety.It is unrestricted on the usage quantity that China is defined in the food, can add by arts demand.
This component of Lai Baodi glucosides Rebaudioside A (RA) is accepted by the human consumer as sweeting agent is the easiest owing to have near the mouthfeel of sucrose, adds the nourishing function that itself possesses, and is expected to promote the use of as high-end sweeting agent.
Steviol glycoside is the terpenes glycoside of a class tool sweet taste, is white powder, and is soluble in water, is insoluble to propylene glycol or ethylene glycol, and water absorbability is strong in air, and mixing with sucrose to use has the effect that multiplies each other significantly.
The traditional extraction process of producing steviol glycoside can be divided into two kinds: a kind of is organic solvent method, directly adopt as ethanol, dioxan equal solvent and extract, but this method solvent consumption is big, and the cost height, practicality is not good enough; Another kind is a water extraction method, water extraction is environmentally friendly, but in the aqueous extract of Folium Chrysanthemi, except that containing stevioside, also there are impurity such as a large amount of organic acids, protein, pigment, inorganic salt, the existence of a large amount of impurity makes the color and luster of extracting solution very dark, brings very big difficulty for the work of separation and refining stevioside.Adopt flocculation that extracting solution is carried out preliminary removal of impurities in traditional steviol glycoside production technique, because flocculation process need add flocculation agent, cause flocculating and contain a large amount of colored ions in the liquid, need spent ion exchange resin to remove, make that entire production process is loaded down with trivial details, the cycle is long, cost is high.And above method inefficiency is extracted repeatedly in order to improve yield, can make extracting liquid volume huge, and unusual difficulty when the solution of water-based concentrates with traditional underpressure distillation mode causes the excessive and increase production cost of energy expenditure.
Summary of the invention
Technical problem to be solved by this invention provides the extraction process of a kind of efficient, Lai Baodi glucosides RA that dna purity is high.For this reason, the present invention is by the following technical solutions: it may further comprise the steps:
(1), pulverize Folium Chrysanthemi,
(2), subcritical water puies forward technology and extracts water-soluble glucosides in the Folium Chrysanthemi, described subcritical water is put forward the processing condition of technology: 120 ~ 180 ℃ of temperature, pressure 1 ~ 6MPa,
(3), to the water-soluble glucosides that extracts with membrane separation technique elimination impurity with concentrate,
(4), macroporous resin adsorption,
(5), the recrystallization separation and purification goes out Lai Baodi glucosides RA.
On the basis of adopting technique scheme, the present invention also can adopt following further technical scheme:
In step (3), at first obtain settled solution by first step membrane filtration, concentrate through second stage membrane filtration again, concentrated solution enters the described macroporous resin adsorption of step (4) and handles.
In step (4) back macroporous resin is obtained the total glycosides solution of sweet Stevia after with ethanol elution, reclaim organic solvent after drying obtain the total glycosides powder of sweet Stevia, then the total glycosides powder of sweet Stevia is carried out the processing of step (5).
In step (5), the solid of need recrystallization is dissolved in the methanol-water solution, concentrate and leave standstill crystallization, isolated crystallization is stevioside St, and Lai Baodi glucosides RA stays in the mother liquor, adds methyl alcohol-alcohol mixeding liquid in mother liquor, stirring, the back is concentrated leaves standstill, stevioside RA crystallization is separated out, and uses ethyl alcohol recrystallization again, the Lai Baodi glucosides RA crystal that obtains.
Owing to adopt technical scheme of the present invention, technology of the present invention is put forward technology with subcritical water and is accelerated the extraction rate of stevioside glycoside material and improved the steviol glycoside solubility rate, more than the total glucosides extraction rate reached to 98% in the raw material, improved the yield of stevioside, rapid extraction goes out the water-soluble glucosides in the sweet Stevia, through membrane separation technique elimination impurity, replace traditional flocculation process, the realization cleaner production can reduce production costs, re-use the further separation and purification of macroporous adsorbent resin and recrystallization technology and go out Lai Baodi glucosides Rebaudioside A (RA), its purity is reached more than 90%.Short, cleaning of a whole set of production technique time, efficient, energy consumption is low.And extracting solution has tangible sweet smell, and the extracting solution of traditional cooking process does not have sweet smell and color darker.
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention.
Embodiment
With reference to accompanying drawing 1, the present invention includes following steps:
(1), pulverize Folium Chrysanthemi,
(2), subcritical water puies forward technology and extracts water-soluble glucosides in the Folium Chrysanthemi, described subcritical water is put forward the processing condition of technology: 120 ~ 180 ℃ of temperature, pressure 1 ~ 6MPa,
(3), to the water-soluble glucosides that extracts with membrane separation technique elimination impurity with concentrate,
(4), absorption with macroporous adsorbent resin,
(5), the recrystallization separation and purification goes out Lai Baodi glucosides RA.
In step (3), at first obtain settled solution by first step membrane filtration, concentrate through second stage membrane filtration again, concentrated solution enters the described absorption with macroporous adsorbent resin of step (4) and handles.
In step (4) back macroporous adsorbent resin is obtained the total glycosides solution of sweet Stevia after with the organic solvent wash-out, drying obtains the total glycosides powder of sweet Stevia behind the recovery organic solvent, then the total glycosides powder of sweet Stevia is carried out the processing of step (5).
In step (5), just need the solid of recrystallization to be dissolved in the methanol-water solution, concentrate and leave standstill crystallization, isolated crystallization is stevioside St, and Lai Baodi glucosides RA stays in the mother liquor, adds methyl alcohol-alcohol mixeding liquid in mother liquor, stirring, the back is concentrated leaves standstill, stevioside RA crystallization is separated out, and uses ethyl alcohol recrystallization again, the Lai Baodi glucosides RA crystal that obtains.
Embodiment 1
Technological operation: after Folium Chrysanthemi (cured leaf, bright leaf all can) blends with pulverizer, drop into extractor, pressurization heats up behind the tap water of 20 times of weight of adding, 140～150 ℃ of temperature, pressure 3～4MPa keeps relief pressure after 30 minutes, obtain settled solution through first step membrane filtration after emitting the extraction liquid naturally cooling, concentrate through second stage membrane filtration again, concentrated solution obtains the total glycosides solution of sweet Stevia behind macroporous resin column absorption, ethanol elution, spraying drying after concentrating under reduced pressure reclaims ethanol promptly gets total glycosides amount at the total glycosides powder of the sweet Stevia more than 95%.The total glycosides powder dissolution of sweet Stevia in methanol-water solution, is concentrated and leaves standstill crystallization, and isolated crystallization is stevioside St, and Lai Baodi glucosides RA stays in the mother liquor.Add methyl alcohol-alcohol mixeding liquid in mother liquor, the back that stirs concentrates leaves standstill, and Lai Baodi glucosides RA crystallization is separated out, and uses ethyl alcohol recrystallization again, and the Lai Baodi glucosides RA crystal purity that obtains is more than 90%.
Described first step membrane filtration can adopt ultrafiltration membrance filter, and described second stage membrane filtration can adopt nanofiltration membrane to filter.
Embodiment 2
Technological operation: every batch of charging capacity of sweet Stevia blade is 30kg, extracts in the small-sized Subcritical Water Extraction jar of 500L, and solid-liquid ratio is 1:10, and extracting temperature is 140～150 ℃, and pressure is 3～4MPa, and extraction time is 30 minutes.Extracting solution cooling is after molecular weight cut-off is to obtain settled solution after 10000 the ultrafiltration membrance filter removal of impurities, be that 100～500 nanofiltration membrane concentrates through molecular weight cut-off again, with the AB-8 macroporous adsorbent resin stevioside glycoside material in the concentrated solution is adsorbed, after 70% ethanolic soln desorb, obtain steviol glycoside solution, spraying drying can obtain the total glycosides powder of faint yellow stevioside after reclaiming ethanol, and total glucosides content is more than 95%.With the total glycosides powder dissolution of sweet Stevia in 60% methanol solution, concentrate and leave standstill crystallization, isolated crystallization is stevioside St, in mother liquor, add methyl alcohol-alcohol mixeding liquid (methyl alcohol: ethanol=1:2), stirring, the back is concentrated leaves standstill, stevioside RA crystallization is separated out, and uses ethyl alcohol recrystallization again, and the stevioside RA crystal purity that obtains is 95.2%.Through lab scale experimental verification repeatedly, from 30kg sweet Stevia blade, can extract the total glucosides amount of 2.10～2.45kg at the total glycosides powder of the sweet Stevia more than 95%, can obtain 0.70～0.85kg purity at the Lai Baodi glucosides RA crystal more than 90% through recrystallizing and refining.
Embodiment 3
Technological operation: after dried sweet Stevia blade blends with pulverizer, drop into extractor, pressurization heats up behind the tap water of 25 times of weight of adding, 140～150 ℃ of temperature, pressure 3～4MPa keeps relief pressure after 40 minutes, obtain the Vandyke brown settled solution through first step micro-filtrate membrane filtration after emitting the extraction liquid naturally cooling, concentrate film again concentrates through the second stage, concentrated solution adsorbs through macroporous resin column AB-8, obtain the total glycosides solution of sweet Stevia behind 70% ethanol elution, spraying drying after concentrating under reduced pressure reclaims ethanol, promptly get the total glycosides powder of faint yellow sweet Stevia, total glycosides content is more than 90%, and yield is 8.5%.
Embodiment 4
Technological operation: directly the bright leaf of sweet Stevia is dropped into extractor, pressurization heats up behind the tap water of 15 times of weight of adding, 140～150 ℃ of temperature, pressure 3～4MPa keeps relief pressure after 50 minutes, obtain the Vandyke brown settled solution through first step micro-filtrate membrane filtration after emitting the extraction liquid naturally cooling, concentrate film again concentrates through the second stage, concentrated solution adsorbs through macroporous resin column AB-8, obtain the total glycosides solution of sweet Stevia behind 70% ethanol elution, spraying drying after concentrating under reduced pressure reclaims ethanol, promptly get the total glycosides powder of faint yellow sweet Stevia, total glycosides content is more than 90%, and yield is 2.8%.
Embodiment 5
Technological operation: with the total glycosides powder dissolution of sweet Stevia in 70% methanol solution, concentrate and leave standstill crystallization, isolated crystallization is stevioside St, in mother liquor, add methyl alcohol-alcohol mixeding liquid (methyl alcohol: ethanol=1:1), stirring, the back is concentrated leaves standstill, Lai Baodi glucosides RA crystallization is separated out, and uses ethyl alcohol recrystallization again, and the Lai Baodi glucosides RA crystal purity that obtains is 91.5%.
Embodiment 6
Technological operation: with the total glycosides powder dissolution of sweet Stevia in 60% methanol solution, concentrate and leave standstill crystallization, isolated crystallization is stevioside St, in mother liquor, add methyl alcohol-alcohol mixeding liquid (methyl alcohol: ethanol=1:2), stirring, the back is concentrated leaves standstill, Lai Baodi glucosides RA crystallization is separated out, and uses ethyl alcohol recrystallization again, and the Lai Baodi glucosides RA crystal purity that obtains is 95.2%.
Claims (4)
1. the extraction process of Yi Zhong Lai Baodi glucosides RA is characterized in that it may further comprise the steps:
(1), pulverize Folium Chrysanthemi,
(2), subcritical water puies forward technology and extracts water-soluble glucosides in the Folium Chrysanthemi, described subcritical water is put forward the processing condition of technology: 120 ~ 180 ℃ of temperature, pressure 1 ~ 6MPa,
(3), to the water-soluble glucosides that extracts with membrane separation technique elimination impurity with concentrate,
(4), macroporous resin adsorption,
(5), the recrystallization separation and purification goes out Lai Baodi glucosides RA.
2. the extraction process of a kind of steviol glycoside RA as claimed in claim 1, it is characterized in that in step (3), at first obtain settled solution by first step membrane filtration, concentrate through second stage membrane filtration, concentrated solution enters the described macroporous resin adsorption of step (4) and handles.
3. the extraction process of a kind of steviol glycoside RA as claimed in claim 2, it is characterized in that macroporous resin being obtained the total glycosides solution of sweet Stevia after with ethanol elution in step (4) back, drying obtains the total glycosides powder of sweet Stevia after reclaiming organic solvent, then the total glycosides powder of sweet Stevia is carried out the processing of step (5).
4. the extraction process of a kind of steviol glycoside RA as claimed in claim 3, it is characterized in that in step (5), the solid of need recrystallization is dissolved in the methanol-water solution, concentrates and leave standstill crystallization, isolated crystallization is stevioside St, Lai Baodi glucosides RA stays in the mother liquor, add methyl alcohol-alcohol mixeding liquid in mother liquor, the back that stirs concentrates leaves standstill, and stevioside RA crystallization is separated out, use ethyl alcohol recrystallization again, the Lai Baodi glucosides RA crystal that obtains.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
| CN104096381A (en) * | 2014-07-09 | 2014-10-15 | 郑州大学 | Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid |
| CN104262428A (en) * | 2014-10-17 | 2015-01-07 | 南通海天生物科技有限公司 | Method for extracting and separating rebaudioside-A from stevia rebaudian leaves |
| CN105246359A (en) * | 2013-05-07 | 2016-01-13 | 泰顿生物科学有限公司 | Green process to hydrolyze carbohydrates from tobacco biomass using subcritical water |
| CN107163090A (en) * | 2017-05-04 | 2017-09-15 | 广东冠龙生物科技有限公司 | A kind of extracting method 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 |
| CN111548378A (en) * | 2020-05-21 | 2020-08-18 | 中国药科大学 | Method for purifying stevioside |
| CN113201035A (en) * | 2021-04-26 | 2021-08-03 | 四川大学 | Method for extracting and separating stevioside from stevia rebaudiana Bertoni by using low co-soluble solvent (DES) |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105246359A (en) * | 2013-05-07 | 2016-01-13 | 泰顿生物科学有限公司 | Green process to hydrolyze carbohydrates from tobacco biomass using subcritical water |
| CN105246359B (en) * | 2013-05-07 | 2018-06-08 | 泰顿生物科学有限公司 | The friendly process of carbohydrate is hydrolyzed from tobacco biomass using subcritical water |
| CN103408614A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Novel preparation technique of steviosin and Rebaudioside-A |
| CN104096381A (en) * | 2014-07-09 | 2014-10-15 | 郑州大学 | Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid |
| CN104096381B (en) * | 2014-07-09 | 2017-05-17 | 郑州大学 | Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid |
| CN104262428A (en) * | 2014-10-17 | 2015-01-07 | 南通海天生物科技有限公司 | Method for extracting and separating rebaudioside-A from stevia rebaudian leaves |
| 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 |
| CN107163090A (en) * | 2017-05-04 | 2017-09-15 | 广东冠龙生物科技有限公司 | A kind of extracting method of stevioside |
| CN111548378A (en) * | 2020-05-21 | 2020-08-18 | 中国药科大学 | Method for purifying stevioside |
| CN113201035A (en) * | 2021-04-26 | 2021-08-03 | 四川大学 | Method for extracting and separating stevioside from stevia rebaudiana Bertoni by using low co-soluble solvent (DES) |
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