CN102827134A - Method for extracting miroestrol from Pueraria Mirifica - Google Patents
Method for extracting miroestrol from Pueraria Mirifica Download PDFInfo
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- CN102827134A CN102827134A CN 201210350673 CN201210350673A CN102827134A CN 102827134 A CN102827134 A CN 102827134A CN 201210350673 CN201210350673 CN 201210350673 CN 201210350673 A CN201210350673 A CN 201210350673A CN 102827134 A CN102827134 A CN 102827134A
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- miroestrol
- extracting
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- tai
- ethanol
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- RJKLDOLOCIQYFS-PRTISISMSA-N miroestrol Chemical compound C12=COC3=CC(O)=CC=C3[C@H]2C(C)(C)[C@@H]2[C@@H]([C@H]3O)[C@@]1(O)C(=O)C[C@]3(O)C2 RJKLDOLOCIQYFS-PRTISISMSA-N 0.000 title claims abstract description 23
- CKEZIBBDMDFHQQ-ILKNQKGPSA-N miroestrol Natural products CC1(C)[C@H]2C[C@]3(O)CC(=O)[C@H]([C@@H]2[C@H]3O)C4=COc5ccccc5[C@@H]14 CKEZIBBDMDFHQQ-ILKNQKGPSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 241001629703 Pueraria candollei var. mirifica Species 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000010828 elution Methods 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 244000046146 Pueraria lobata Species 0.000 description 5
- 235000010575 Pueraria lobata Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000284 extract Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 210000000038 chest Anatomy 0.000 description 3
- 239000000262 estrogen Substances 0.000 description 3
- 229940011871 estrogen Drugs 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000002124 endocrine Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000290333 Vanilla fragrans Species 0.000 description 1
- 235000009499 Vanilla fragrans Nutrition 0.000 description 1
- 235000012036 Vanilla tahitensis Nutrition 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000001076 estrogenic effect Effects 0.000 description 1
- 239000002024 ethyl acetate extract Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- -1 flavonoid compound Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036449 good health Effects 0.000 description 1
- CJWQYWQDLBZGPD-UHFFFAOYSA-N isoflavone Natural products C1=C(OC)C(OC)=CC(OC)=C1C1=COC2=C(C=CC(C)(C)O3)C3=C(OC)C=C2C1=O CJWQYWQDLBZGPD-UHFFFAOYSA-N 0.000 description 1
- 150000002515 isoflavone derivatives Chemical class 0.000 description 1
- 235000008696 isoflavones Nutrition 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 239000003075 phytoestrogen Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for extracting miroestrol from Pueraria Mirifica, which comprises the following steps: 1) pulverizing Pueraria Mirifica, adding 3-10 times of 30-90 percent ethanol solution, extracting under reflux 2-3 times, recycling the reagent from the extracting solution, adsorbing with a macroporous resin, carrying out gradient elution with an ethanol solution, concentrating the eluate under reduced pressure, and standing to crystallize; and 2) dissolving the crystals in ethanol, adding the solution into a polyamide resin, drying, filling into a column, carrying out gradient elution with ethanol, carrying out thin-layer detection, collecting the target fraction, concentrating the fraction to small volume to crystallize, and drying to obtain the miroestrol. The method disclosed by the invention is simple to operate and suitable for industrial production, and a single reagent is used.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of method of from Tai Gegen, extracting Miroestrol.
Background technology
Thailand's root (Pueraria Mirifica) has another name called white height (white Kwao Krua); Being the tropical vanilla of a kind of mystery of Thailand, also being commonly called as the breast fruit, is the rare protective plant of Thailand; Be grown in the northern virgin forest of Thailand, the root piece is grown in underground 1-2 rice depths.Pueraria Mirifica is northern just as women's folk tradition secret recipe food in Thailand since ancient times, can make female chest plentiful, and the figure is beautiful, and the colour of skin is pale, has good health and a long life.The scientific research result finds: the wild root of kudzu vine that grows in Thailand's Mountainous Area of North contain abundant have similar female estrogen effect, the effective high reactivity NOVASOY 400 of endocrine regulation; Its activity is more than 1,000 times of soybean isoflavones, simulates and disturb estrogenic Physiology and biochemistry effect more remarkable.Therefore, to regulating the female incretion level, the effect of effectively alleviating estrogen relative diseases is particularly evident.This conclusion is that passing on from generation to generation of Pueraria Mirifica is used to chest enlarge, endocrine regulation and delays senility found scientific basis.Different with other leguminous plants is its distinctive " Miroestrol " and vegetable active compositions such as " the little female alcohol of deoxidation "; These activeconstituentss are that other leguminous plantss do not have; Sp act composition in the safe root of kudzu vine; Increase and grow for women's chest and be of miraculous efficacy, thereby make it unusual and praised highly by professional medical mechanism and SPA.
Miroestrol (Miroestrol) is a flavonoid compound, molecular formula C
20H
22O
6, molecular weight 358.39, molecular structural formula:
Miroestrol is colourless rectangle sheet crystallization (anhydrous methanol), 268～270 ℃ of fusing points (decomposition), and Miroestrol has very strong estrogen effect.
Through literature search, from Tai Gegen, extract the method for Miroestrol, domestic research is less.Be that the method for mentioning is the Pueraria Mirifica drying and crushing in the document " phytoestrogen in the Thailand elegant jessamine---deoxidation Miroestrol ", in apparatus,Soxhlet's, extract 10h with hexane, ETHYLE ACETATE and ethanol successively, ethyl acetate extract is through silica gel column chromatography.This kind method is comparatively loaded down with trivial details, uses multiple easy volatile solvent, is not suitable for industriallization, is necessary so a kind of industrial method that from Tai Gegen, extracts Miroestrol is provided.
Summary of the invention
The present invention aims to provide a kind of industrial method that from Tai Gegen, extracts Miroestrol.
The objective of the invention is to realize through following technical scheme:
A kind of method of from Tai Gegen, extracting Miroestrol is characterized in that following steps:
1) get Tai Gegen and pulverize, add 3-10 and doubly measure 30-90% ethanolic soln refluxing extraction 2-3 time, extracting solution is used macroporous resin adsorption after reclaiming reagent, the ethanolic soln gradient elution, and the elutriant concentrating under reduced pressure is placed crystallization;
2) above-mentioned crystallisate is adorned post after adding the polyamide resin drying with dissolve with ethanol, uses the ethanolic soln gradient elution again, and thin layer detects, and collects the target flow point, and flow point is concentrated into the small volume crystallization, is drying to obtain.
Optional polar macroporous resin of macroporous resin described in the step 1) or non-polar macroporous resin, a kind of among the optional D101 of model, AB-8 or the ADS-21.
Ethanolic soln gradient elution described in the step 1) is: earlier with 4-8 times of column volume 10-40% ethanol elution impurity, again with 3-6 times of column volume 50-80% ethanol elution effective constituent.
Step 2) polyamide resin described in is a granularity 120-200 order polyamide resin, and consumption is 5-20 a times of applied sample amount.
Step 2) the ethanolic soln gradient elution described in is: earlier with 5-10 times of column volume 10-20% ethanol elution impurity, use 30-50% ethanol elution target component again.
Advantage of the present invention is that method adopts macroporous resin adsorption and polyamide resin united purification, and simple to operate, reagent is single and treatment capacity is big, is easy to industriallization.
Embodiment:
To combine embodiment to further specify the present invention below.
Embodiment 1:
The safe root of kudzu vine is pulverized, and takes by weighing 10kg and adds 3 times of amount 90% ethanolic soln refluxing extraction 3 times, and extracting solution is used the D101 macroporous resin adsorption after reclaiming reagent; Earlier with 8 times of column volumes, 10% ethanol elution impurity; Use 4 times of column volumes, 50% ethanol elution effective constituent again, the elutriant concentrating under reduced pressure is placed crystallization.Crystallisate leaches with adorning post after the 90% dissolve with ethanol adding 1kg polyamide resin drying, with 10L10% ethanol elution impurity, uses 30% ethanol elution target component again; Thin layer detects; Collect the target flow point, flow point is concentrated into the small volume crystallization, is drying to obtain white crystals Miroestrol 11g.
Embodiment 2:
The safe root of kudzu vine is pulverized, and takes by weighing 10kg and adds 7 times of amount 50% ethanolic soln refluxing extraction 2 times, and extracting solution is used the AB-8 macroporous resin adsorption after reclaiming reagent; Earlier with 5 times of column volumes, 40% ethanol elution impurity; Use 3 times of column volumes, 80% ethanol elution effective constituent again, the elutriant concentrating under reduced pressure is placed crystallization.Crystallisate leaches with adorning post after the 95% dissolve with ethanol adding 1kg polyamide resin drying, with 8L20% ethanol elution impurity, uses 50% ethanol elution target component again; Thin layer detects; Collect the target flow point, flow point is concentrated into the small volume crystallization, is drying to obtain white crystals Miroestrol 17g.
Embodiment 3:
The safe root of kudzu vine is pulverized, and takes by weighing 10kg and adds 5 times of amount 60% ethanolic soln refluxing extraction 3 times, and extracting solution is used the ADS-21 macroporous resin adsorption after reclaiming reagent; Earlier with 4 times of column volumes, 30% ethanol elution impurity; Use 5 times of column volumes, 60% ethanol elution effective constituent again, the elutriant concentrating under reduced pressure is placed crystallization.Crystallisate leaches with adorning post after the 90% dissolve with ethanol adding 1kg polyamide resin drying, with 7L20% ethanol elution impurity, uses 40% ethanol elution target component again; Thin layer detects; Collect the target flow point, flow point is concentrated into the small volume crystallization, is drying to obtain white crystals Miroestrol 15g.
Claims (5)
1. method of from Tai Gegen, extracting Miroestrol is characterized in that following steps:
1) get Tai Gegen and pulverize, add 3-10 and doubly measure 30-90% ethanolic soln refluxing extraction 2-3 time, extracting solution is used macroporous resin adsorption after reclaiming reagent, the ethanolic soln gradient elution, and the elutriant concentrating under reduced pressure is placed crystallization;
2) above-mentioned crystallisate is adorned post after adding the polyamide resin drying with dissolve with ethanol, uses the ethanolic soln gradient elution again, and thin layer detects, and collects the target flow point, and flow point is concentrated into the small volume crystallization, is drying to obtain.
2. the method for from Tai Gegen, extracting Miroestrol according to claim 1 is characterized in that optional polar macroporous resin of the macroporous resin described in the step 1) or non-polar macroporous resin, a kind of among the optional D101 of model, AB-8 or the ADS-21.
3. the method for from Tai Gegen, extracting Miroestrol according to claim 1; It is characterized in that the ethanolic soln gradient elution described in the step 1) is: earlier with 4-8 times of column volume 10-40% ethanol elution impurity, again with 3-6 times of column volume 50-80% ethanol elution effective constituent.
4. the method for from Tai Gegen, extracting Miroestrol according to claim 1 is characterized in that step 2) described in polyamide resin be granularity 120-200 order polyamide resin, consumption be applied sample amount 5-20 doubly.
5. the method for from Tai Gegen, extracting Miroestrol according to claim 1 is characterized in that step 2) described in the ethanolic soln gradient elution be: earlier with 5-10 times of column volume 10-20% ethanol elution impurity, use 30-50% ethanol elution target component again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210350673 CN102827134A (en) | 2012-09-20 | 2012-09-20 | Method for extracting miroestrol from Pueraria Mirifica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210350673 CN102827134A (en) | 2012-09-20 | 2012-09-20 | Method for extracting miroestrol from Pueraria Mirifica |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102827134A true CN102827134A (en) | 2012-12-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210350673 Pending CN102827134A (en) | 2012-09-20 | 2012-09-20 | Method for extracting miroestrol from Pueraria Mirifica |
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| CN (1) | CN102827134A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625021A (en) * | 2019-09-24 | 2021-04-09 | 粉嫩公主生物科技有限公司 | Method for purifying puerarin by two-dimensional preparation liquid chromatography |
-
2012
- 2012-09-20 CN CN 201210350673 patent/CN102827134A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625021A (en) * | 2019-09-24 | 2021-04-09 | 粉嫩公主生物科技有限公司 | Method for purifying puerarin by two-dimensional preparation liquid chromatography |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121219 |