CN103570789A - Preparation method of high-purity momordica glycosides - Google Patents
Preparation method of high-purity momordica glycosides Download PDFInfo
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- CN103570789A CN103570789A CN201310563800.XA CN201310563800A CN103570789A CN 103570789 A CN103570789 A CN 103570789A CN 201310563800 A CN201310563800 A CN 201310563800A CN 103570789 A CN103570789 A CN 103570789A
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Abstract
The invention relates to a preparation method of high-purity momordica glycosides. The preparation method comprises the following steps: extracting momordica grosvenori; concentrating to prepare an extract; carrying out two phase liquid-liquid extraction on a mixed liquid of ethyl ether and ethyl acetate; carrying out two aqueous phase liquid-liquid extraction on a mixed liquid of ethanol and ethyl acetate/dipotassium phosphate; carrying out reverse extraction on a high-molecular polymer, namely polyacrylamide; carrying out two phase liquid-liquid extraction on organic solvent n-butyl alcohol; concentrating; and drying; in the preparation method, the two phase liquid-liquid extraction and the two aqueous phase liquid-liquid extraction are carried out.
Description
Technical field
The invention belongs to plant milk extract technical field, relate to a kind of preparation method of high-purity Momordica grosvenori mogroside.
Background technology
Grosvenor Momordica is Guangxi characteristic medicine-food two-purpose cash crop, contains Momordica-Glycosides in fruit, and its heat is zero, and the effect that have clearing heat and moistening lung antibechic, relaxes bowel, has preventive and therapeutic effect to obesity, constipation, diabetes etc.In Momordica-Glycosides, the sugariness of Momordica grosvenori mogroside V is sucrose 300 times, Momordica-Glycosides is safety non-toxic as food, Grosvenor Momordica is sweet can be quantity-unlimiting for varieties of food items.Fructus Monordicae extract is not only applied to, in pharmaceutical industries, in fields such as food, all be widely used.The preparation of existing Momordica-Glycosides mainly obtains by methods such as column chromatography or membrane filtrations, and its production cycle is long, and cost is higher, large on the impact of environment.The present invention relates to a double water-phase method simple, that efficiency is high, yield is high and purity is high and prepare Momordica-Glycosides, suitability for industrialized is produced.
Summary of the invention
The object of the invention is to disclose a kind of preparation method of high-purity Momordica grosvenori mogroside.
Technical scheme of the present invention is: a kind of preparation method of high-purity Momordica grosvenori mogroside, take fresh Fructus Momordicae as raw material, take ethanol and water mixed liquid prepares Grosvenor Momordica extracting solution as solvent, extracting solution concentrates to obtain medicinal extract, medicinal extract is water-soluble, fat-soluble organic solvent two-phase extraction, add organic solvent mixed solution and salt formation aqueous two-phase system, by aqueous two-phase system abstraction purification, high molecular weight water soluble polymer optionally extracting and separating, select the good organic solvent enrichment Momordica-Glycosides of Momordica-Glycosides affinity, complete the total sweet glucoside of separated separation and purification Grosvenor Momordica from medicinal extract.
The preparation method of a kind of high-purity Momordica grosvenori mogroside of the present invention comprises that Grosvenor Momordica extracts-be condensed into the operations such as medicinal extract-ether, ethyl acetate mixed solution two-phase liquid-liquid extraction-ethanol, the liquid-liquid extraction of ethyl acetate mixed solution/dipotassium hydrogen phosphate double water-phase liquid-liquid extraction-macromolecule copolymer polyacrylamide back extraction-organic solvent propyl carbinol two-phase-concentrated-dry, comprising two-phase liquid-liquid extraction, double water-phase liquid-liquid extraction.Concrete operation step is as follows:
1. water extraction: Grosvenor Momordica is pulverized and added in extraction equipment, in the ratio of raw material and water weight ratio 1:6, add water, under 90-100 ℃ of condition, extract three times, 1-2 hour at every turn, united extraction liquid, concentrating under reduced pressure becomes medicinal extract.
2. medicinal extract step 1 being obtained is water-soluble, adds the ether of same volume: ethyl acetate mixeding liquid volume, than for 7:3, extracts 3-4 time, is extracted the aqueous solution of rear enrichment Momordica-Glycosides.
3. by the step 2 gained Momordica-Glycosides aqueous solution, add aqueous solution weight 10% dipotassium hydrogen phosphate solid, add same volume ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, extracts 3-4 time, combining extraction liquid, the Momordica-Glycosides in the aqueous solution is enriched to ethanol, ethyl acetate mixed solution.
4. the polyacrylamide solution that is 1%-1.5% by the mass percent of step 3 gained ethanol, ethyl acetate mixed solution and same volume is stripped once, and ethanol, ethyl acetate mixed solution evaporated under reduced pressure, obtain crude product Momordica-Glycosides.
Step 4 gained crude product Momordica-Glycosides is water-soluble 5., by the aqueous solution: propyl carbinol volume ratio 2:1 adds propyl carbinol, extracts 5-6 time, collect propyl carbinol liquid evaporated under reduced pressure, obtain the total sweet glucoside of Grosvenor Momordica, purity reaches more than 95%, Momordica grosvenori mogroside V, purity reaches more than 65%.
In above step 2, add the ether of same volume: ethyl acetate mixeding liquid volume, than for 7:3, extracts 3 times.
In above step 4, in polyacrylamide solution, polyacrylamide mass percent is 1%.
In above step 5, the aqueous solution: propyl carbinol volume ratio 2:1, extracts 6 times.
Feature of the present invention is:
The preparation method of high-purity Momordica grosvenori mogroside of the present invention, utilizes ether and ethyl acetate mixed solution to carry out two-phase extraction and removes lipid-soluble substance; Utilize ethanol, ethyl acetate mixed solution/dipotassium hydrogen phosphate to form two phase aqueous extraction system; Utilization has the macromolecule copolymer polyacrylamide back extraction enrichment Momordica-Glycosides of selective extraction; Select the good organic solvent propyl carbinol enrichment Momordica-Glycosides of Momordica-Glycosides affinity, through extraction and back-extraction repeatedly, after getting, obtain the above high-purity Momordica grosvenori mogroside of weight content 95%.It is large that the method has treatment capacity, and technical process is short, can carry out operate continuously, advantage that separation efficiency is high, and be homogeneous system, is easy to continuous production operation.
Specific embodiments
Embodiment mono-:
Take Grosvenor Momordica fresh fruit 500g, fragmentation, adds in extraction equipment, adds 3000g reverse osmosis water, under 100 ℃ of conditions, repeatedly extract three times, and each 2 hours, united extraction liquid, concentrating under reduced pressure becomes medicinal extract.Medicinal extract is dissolved in and in reverse osmosis water, is made into the 500ml aqueous solution, add 500ml ether: ethyl acetate mixeding liquid volume is than being 7:3, extract 3 times, combining extraction liquid reclaims, in the extraction aqueous solution later, add aqueous solution weight 50g dipotassium hydrogen phosphate, add again 500ml ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, concussion, standing, form double water-phase, obtain is ethanol mutually, ethyl acetate hybrid extraction liquid, the mass percent of hybrid extraction liquid and 500ml is that 1% polyacrylamide solution is stripped once, ethanol, ethyl acetate mixed solution evaporated under reduced pressure, obtain yellow crude product Momordica-Glycosides, gained crude product Momordica-Glycosides is water-soluble, molten by the aqueous solution: propyl carbinol volume ratio 2:1 adds propyl carbinol, extract 6 times, collect propyl carbinol liquid evaporated under reduced pressure, obtain the total sweet glucoside of Grosvenor Momordica, with determined by ultraviolet spectrophotometry, the total sweet glucoside weight content of Grosvenor Momordica is 96%, with high effective liquid chromatography for measuring, Momordica grosvenori mogroside V weight content is 68%.
Embodiment bis-:
Take Grosvenor Momordica fresh fruit 500g, fragmentation, adds in extraction equipment, adds 3000g reverse osmosis water, under 100 ℃ of conditions, repeatedly extract three times, and each 1 hour, united extraction liquid, concentrating under reduced pressure becomes medicinal extract.Medicinal extract is dissolved in and in reverse osmosis water, is made into the 500ml aqueous solution, add 500ml ether: ethyl acetate mixeding liquid volume is than being 7:3, extract 4 times, combining extraction liquid reclaims, in the extraction aqueous solution later, add aqueous solution weight 50g dipotassium hydrogen phosphate, add again 500ml ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, concussion, standing, form double water-phase, obtain is ethanol mutually, ethyl acetate hybrid extraction liquid, the mass percent of hybrid extraction liquid and 500ml is that 1.5% polyacrylamide solution is stripped once, ethanol, ethyl acetate mixed solution evaporated under reduced pressure, obtain yellow crude product Momordica-Glycosides, gained crude product Momordica-Glycosides is water-soluble, molten by the aqueous solution: propyl carbinol volume ratio 2:1 adds propyl carbinol, extract 5 times, collect propyl carbinol liquid evaporated under reduced pressure, obtain the total sweet glucoside of Grosvenor Momordica, with determined by ultraviolet spectrophotometry, the total sweet glucoside weight content of Grosvenor Momordica is 95%, with high effective liquid chromatography for measuring, Momordica grosvenori mogroside V weight content is 65%.
Embodiment tri-:
Take Grosvenor Momordica fresh fruit 500g, fragmentation, adds in extraction equipment, adds 3000g reverse osmosis water, under 100 ℃ of conditions, repeatedly extract three times, and each 1 hour, united extraction liquid, concentrating under reduced pressure becomes medicinal extract.Medicinal extract is dissolved in and in reverse osmosis water, is made into the 500ml aqueous solution, add 500ml ether: ethyl acetate mixeding liquid volume is than being 7:3, extract 3 times, combining extraction liquid reclaims, in the extraction aqueous solution later, add aqueous solution weight 50g dipotassium hydrogen phosphate, add again 500ml ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, concussion, standing, form double water-phase, obtain is ethanol mutually, ethyl acetate hybrid extraction liquid, the mass percent of hybrid extraction liquid and 500ml is that 1.5% polyacrylamide solution is stripped once, ethanol, ethyl acetate mixed solution evaporated under reduced pressure, obtain yellow crude product Momordica-Glycosides, gained crude product Momordica-Glycosides is water-soluble, molten by the aqueous solution: propyl carbinol volume ratio 2:1 adds propyl carbinol, extract 5 times, collect propyl carbinol liquid evaporated under reduced pressure, obtain the total sweet glucoside of Grosvenor Momordica, with determined by ultraviolet spectrophotometry, the total sweet glucoside weight content of Grosvenor Momordica is 96%, with high effective liquid chromatography for measuring, Momordica grosvenori mogroside V weight content is 66%.
Claims (5)
1. the preparation method of a high-purity Momordica grosvenori mogroside, it is characterized in that: production process comprises Grosvenor Momordica water extraction-be condensed into medicinal extract-ether, ethyl acetate mixed solution two-phase liquid-liquid extraction-ethanol, ethyl acetate mixed solution/dipotassium hydrogen phosphate double water-phase liquid-liquid extraction-macromolecule copolymer polyacrylamide back extraction-organic solvent propyl carbinol two-phase liquid-liquid extraction-concentrated-dry, and its operational process of craft is:
1) water extraction: Grosvenor Momordica is pulverized and added in extraction equipment, in the ratio of raw material and water weight ratio 1:6, add water, 90-100 ℃ of condition, can descend to extract three times, each 1-2 hour, united extraction liquid, concentrating under reduced pressure becomes medicinal extract.
2) by step 1) medicinal extract that obtains is water-soluble, adds the ether of same volume: ethyl acetate mixeding liquid volume, than being 7:3, extracts 3-4 time, is extracted the aqueous solution of rear enrichment Momordica-Glycosides.
3) by step 2) the gained Momordica-Glycosides aqueous solution, add aqueous solution weight 10% dipotassium hydrogen phosphate solid, add same volume ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, extract 3-4 time, combining extraction liquid, the Momordica-Glycosides in the aqueous solution is enriched to ethanol, ethyl acetate mixed solution.
4) by step 3) mass percent of gained ethanol, ethyl acetate mixed solution and same volume is 1%-1.5% polyacrylamide solution is stripped once, ethanol, ethyl acetate mixed solution evaporated under reduced pressure, obtain crude product Momordica-Glycosides.
5) by step 4) gained crude product Momordica-Glycosides is water-soluble, by the aqueous solution: propyl carbinol volume ratio 2:1 adds propyl carbinol, extracts 5-6 time, collect propyl carbinol liquid evaporated under reduced pressure, obtain the total sweet glucoside of Grosvenor Momordica, purity reaches more than 95%, Momordica grosvenori mogroside V, purity reaches more than 65%.
2. the preparation method of a kind of high-purity Momordica grosvenori mogroside according to claim 1, is characterized in that: step 2) ether: ethyl acetate mixeding liquid volume, than for 7:3, extracts 3 times.
3. the preparation method of a kind of high-purity Momordica grosvenori mogroside according to claim 1, is characterized in that: step 3) ethanol: the mixed solution that ethyl acetate volume ratio is 9:1, extracts 3 times.
4. the preparation method of a kind of high-purity Momordica grosvenori mogroside according to claim 1, is characterized in that: step 4) polyacrylamide mass percent is 1% in polyacrylamide solution, back extraction 1 time.
5. the preparation method of a kind of high-purity Momordica grosvenori mogroside according to claim 1, is characterized in that: step 5) aqueous solution: propyl carbinol volume ratio 2:1, extracts 6 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530168A (en) * | 2014-12-12 | 2015-04-22 | 黄晓 | Industrialization preparation method of mogroside V |
| CN106967142A (en) * | 2017-03-30 | 2017-07-21 | 湖南华诚生物资源股份有限公司 | It is a kind of at the same extract momordica glycoside V, VI and 11 O base glycosides V method |
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| CN101050230A (en) * | 2006-04-07 | 2007-10-10 | 广州泽力医药科技有限公司 | Extraction and preparation process of momordica grosvenori extract |
| CN102697839A (en) * | 2012-06-01 | 2012-10-03 | 武汉工程大学 | Aqueous two-phase extraction and separation method for flavonoids, saponins and polysaccharides of astragalus |
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Patent Citations (2)
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| CN101050230A (en) * | 2006-04-07 | 2007-10-10 | 广州泽力医药科技有限公司 | Extraction and preparation process of momordica grosvenori extract |
| CN102697839A (en) * | 2012-06-01 | 2012-10-03 | 武汉工程大学 | Aqueous two-phase extraction and separation method for flavonoids, saponins and polysaccharides of astragalus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530168A (en) * | 2014-12-12 | 2015-04-22 | 黄晓 | Industrialization preparation method of mogroside V |
| CN106967142A (en) * | 2017-03-30 | 2017-07-21 | 湖南华诚生物资源股份有限公司 | It is a kind of at the same extract momordica glycoside V, VI and 11 O base glycosides V method |
| CN106967142B (en) * | 2017-03-30 | 2019-07-02 | 湖南华诚生物资源股份有限公司 | Method that is a kind of while extracting momordica glycoside V, VI and 11-O base glycosides V |
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Application publication date: 20140212 |