CN1045967C - Method for prepn. of Rhizoma Bolbostemmatis methyl saponin - Google Patents
Method for prepn. of Rhizoma Bolbostemmatis methyl saponin Download PDFInfo
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- CN1045967C CN1045967C CN93110381A CN93110381A CN1045967C CN 1045967 C CN1045967 C CN 1045967C CN 93110381 A CN93110381 A CN 93110381A CN 93110381 A CN93110381 A CN 93110381A CN 1045967 C CN1045967 C CN 1045967C
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- total
- tubeimoside
- tubeimosides
- water
- saponin
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Abstract
A traditional Chinese medicinal material, rhizoma bolbostemmae, is pulverized, processed by diluted alcohol lixiviation, concentrated, diluted with water, extracted by water saturated C4-C5 fatty alcohol and steamed to remove solvents, so that total rhizoma bolbostemmae saponins are obtained; the saponins dissolve in methanol, and the mixed solvents are precipitated so as to obtain the crude product of rhizoma bolbostemmae saponin A; or the total saponins dissolve in hot water, are processed by macroporous polymeric resin laminar analysis, eluted by diluted alcohol; then the mixed solvents are precipitated, so that the crude product of rhizoma bolbostemmae saponin A is obtained. After refined by methanol containing water and mixed-solvent process, the solvents with the advantages of low price, easy acquirement, little toxicity, convenient technology, simple equipment and low cost are suitable for national conditions and can be put into industrial production.
Description
The present invention relates to vegetable drug and extract, separate category, particularly the method for therefrom extracting and separating tubeimoside first element in the sphragidite bulb of fritillary.
Cucurbitaceous plant Rhizome of Paniculate Bolbostemma (Bolbostemma paniculatum (Maxim.) Fran-quet), the property hardship is slightly cold.The function dissipating bind, detumescence, detoxifcation.The traditional Chinese medical science is used for the treatment of acute mastitis scrofula, mazoitis, lymphoid tuberculosis, chronic lymphadenitis, hypertrophic rhinitis etc.
From the Total Tubeimosides of its extraction, isolate multiple triterpenoid saponin and steroid saponin composition, wherein, tubeimoside first element (Tubeimoside I), molecular formula is C
63H
98O
29, structural formula is:
Known it have anti-inflammatory, anticancer and anti-promoting physiological activity.
The extraction and the separation method of tubeimoside first element of the prior art are that pulverizing medicinal materials is become the end, the leaching of 75% ethanol, alcohol is steamed in decompression, water layer after the imitative extraction of surplus liquid chlorine is used n-butanol extraction, separates out Total Tubeimosides after n-butanol extracting liquid concentrating under reduced pressure and the placement.Separate Total Tubeimosides with the silica gel H low pressure column chromatography then, obtain tubeimoside first element.
The deficiencies in the prior art are the chloroform give extraction solvents that need with severe toxicity, separate with liquid chromatograph, and the little cost of output is high, and processing condition can't adapt to the suitability for industrialized production needs.
Purpose of the present invention will be developed a kind of large-batch industrial method of suitable national conditions exactly.
Design of the present invention is implemented with following technical scheme:
Development and design is a kind of to be belonged to vegetable drug and extracts category, comprises pulverizing medicinal materials, solvent lixiviate, concentrates, the preparation method of the tubeimoside first element of steps such as solvent extraction once more, reconcentration, separation, it is characterized in that:
1. at first extract Total Tubeimosides, secondly separate preparation tubeimoside first element,
2. pulverizing medicinal materials to 5～20 orders in≤80 ℃ of lixiviates 2～4 times, boil off solvent with 60～80% ethanol or methyl alcohol, and surplus liquid is concentrated into medicinal extract, after 2～4 times of water gagings dilutions, uses water saturated C
5～C
5Fatty Alcohol(C12-C14 and C12-C18) extraction 2～4 times, extraction liquid pressure reducing and steaming organic solvent, vacuum-drying gets Total Tubeimosides,
3. Total Tubeimosides dissolve with methanol, the mixed solvent precipitation, the plain crude product of tubeimoside first,
4. or the Total Tubeimosides hot water dissolving, macroporous adsorption resin chromatography, rare pure wash-out, the mixed solvent precipitation, the plain crude product of tubeimoside first.
The preparation method of above-mentioned tubeimoside first element, described mixed solvent method precipitation is to point in the methanol solution of Total Tubeimosides, adds acetone, ether or the acetone-ether mixed solution of 2～6 times of amounts.
The preparation method of above-mentioned tubeimoside first element, described macroporous adsorption resin chromatography is meant and uses D
101D
520, models such as AB-8, NKA-II macroporous adsorption resin chromatography.
The preparation method of above-mentioned tubeimoside first element, described rare pure wash-out is meant earlier the ethanol flush away impurity with 25～35%, uses 40～70% ethanol elution tubeimoside first element again.
The preparation method of above-mentioned tubeimoside first element, the plain crude product of described tubeimoside first is refining through the method that aqueous methanol dissolving-mixed solvent settles out.
Compared with prior art, the inventive method has following advantage:
Solvent valency health, be easy to get, toxicity is less;
2. technology is easy, and equipment is simple, and cost is low, is fit to national conditions, can drop into suitability for industrialized production.
Reached intended purposes of the present invention preferably.
The present invention is further elaborated below in conjunction with embodiment:
[embodiment one]
Rhizome of Paniculate Bolbostemma medicinal material 5kg, pulverized 5 mesh sieves, 60% ethanol that with total amount is 20L is in 80 ℃ of lixiviates 2 times, boil off solvent, surplus liquid is concentrated into medicinal extract, after the dilution of 2 times of water gagings, is the water saturated n-butanol extraction 2 times of 6L with total amount, extraction liquid pressure reducing and steaming organic solvent, vacuum-drying gets Total Tubeimosides 0.13kg.
Above-mentioned amount Total Tubeimosides, use the 0.26L dissolve with methanol, in the methanol solution of Total Tubeimosides, add the acetone precipitation of 2 times of amounts, leave standstill 24h, get the plain crude product 0.046kg of tubeimoside first, through aqueous methanol dissolving--the acetone method that settles out is refining, leave standstill 24h, get the plain finished product 0.04kg of white tubeimoside first, yield 0.8%; High performance liquid chromatograph is measured, content 96.5%, 251～252 ℃ of mp.
[embodiment two] Rhizome of Paniculate Bolbostemma medicinal material 5kg, be crushed to 20 orders, with 80% ethanol in 60 ℃ of lixiviates 4 times, boil off solvent, surplus liquid is concentrated into medicinal extract, after 4 times of water gaging dilutions, with the water saturated primary isoamyl alcohol extraction of 20L 4 times, extraction liquid pressure reducing and steaming organic solvent, vacuum-drying gets Total Tubeimosides 0.125kg.
The Total Tubeimosides hot water dissolving uses D
101Or D
520The type macroporous adsorption resin chromatography, 25% ethanol flush away impurity, 40% ethanol elution, reclaim ethanol, drying, the products therefrom dissolve with methanol of 0.1L, to the ether that wherein adds 6 times of amounts, separate out white precipitate, leave standstill 24h, get the plain crude product 0.039kg of tubeimoside first, make with extra care through aqueous methanol dissolving-acetone, the ether mixed solvent method that settles out, leave standstill 24h, get the plain finished product 0.031kg of white tubeimoside first, yield 0.6%; High performance liquid chromatograph is measured, content 95.5%, 249～251 ℃ of mp.
[embodiment three]
Rhizome of Paniculate Bolbostemma medicinal material 55kg, pulverized 10 mesh sieves, with 60% methyl alcohol of total amount 20L in 80 ℃ of lixiviates 2 times, boil off solvent, surplus liquid is concentrated into medicinal extract, after 2 times of water gaging dilutions, uses the water saturated isopropylcarbinol of 5L to extract 2 times, extraction liquid pressure reducing and steaming organic solvent, vacuum-drying gets Total Tubeimosides 0.126kg.
Above-mentioned amount Total Tubeimosides, dissolve with methanol with 0.26L, in the methanol solution of Total Tubeimosides, add the acetone precipitation of 2 times of amounts, leave standstill 24h, get the plain crude product 0.047kg of tubeimoside first, through aqueous methanol dissolving--the acetone method that settles out is refining, leave standstill 24h, get the plain finished product 0.041kg of white tubeimoside first, yield 0.8%; High performance liquid chromatograph is measured, content 95.3%, mp249～251 ℃.
[embodiment four] Rhizome of Paniculate Bolbostemma medicinal material 5kg pulverizes 20 orders, uses 20L80% methyl alcohol in 60 ℃ of lixiviates 4 times, boil off solvent, surplus liquid is concentrated into medicinal extract, extracts 4 times with the water saturated amylalcohol of 5L with 4 times of water gaging dilution backs, extraction liquid pressure reducing and steaming organic solvent, vacuum-drying gets Total Tubeimosides 0.131kg.
The Total Tubeimosides hot water dissolving uses NKA-II or AB-8 type macroporous adsorption resin chromatography, 35% ethanol flush away impurity, 70% ethanol elution reclaims ethanol, drying, products therefrom to the ether that wherein adds 6 times of amounts, is separated out white precipitate with the dissolve with methanol of 0.1L, leave standstill 24h, the plain crude product 0.038kg of tubeimoside first, through the aqueous methanol dissolving--acetone, the ether mixed solvent method that settles out is refining, leaves standstill 24h, get the plain finished product 0.0295kg of white tubeimoside first, yield 0.6%; High performance liquid chromatograph is measured, content 96.4%, 251～252 ℃ of mp.
Claims (1)
1. the preparation method of a tubeimoside first element comprises solvent lixiviate Total Tubeimosides from medicinal material, and preparation tubeimoside first element is separated in the back, it is characterized in that:
After the pulverizing medicinal materials with 60～80% ethanol or methyl alcohol in 60～80 ℃ of lixiviates,
The Total Tubeimosides hot water dissolving, macroporous adsorption resin chromatography, 25～35% ethanol flush away impurity are again through 40～70% ethanol elutions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110381A CN1045967C (en) | 1993-04-07 | 1993-04-07 | Method for prepn. of Rhizoma Bolbostemmatis methyl saponin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110381A CN1045967C (en) | 1993-04-07 | 1993-04-07 | Method for prepn. of Rhizoma Bolbostemmatis methyl saponin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1093272A CN1093272A (en) | 1994-10-12 |
| CN1045967C true CN1045967C (en) | 1999-10-27 |
Family
ID=4988254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93110381A Expired - Fee Related CN1045967C (en) | 1993-04-07 | 1993-04-07 | Method for prepn. of Rhizoma Bolbostemmatis methyl saponin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045967C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038016C (en) * | 1994-11-14 | 1998-04-15 | 万广根 | Wart ointment |
| CN1303097C (en) * | 2004-12-09 | 2007-03-07 | 中国人民解放军第二军医大学 | Japanese polygala saponin kind compound and aglucon, total saponin and total aglucon and its application in medicine |
| CN102603853A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Efficient separation and purification method of tubeimoside |
| CN109336943A (en) * | 2018-10-26 | 2019-02-15 | 宁县恒瑞康生物科技有限公司 | A kind of Bolbostemma paniculatum glucoside A purification process |
| CN111233963B (en) * | 2020-03-02 | 2020-11-13 | 河南中医药大学 | Active monomer for treating esophageal cancer, and composition and application thereof |
| CN116509048A (en) * | 2023-05-10 | 2023-08-01 | 江苏浩丰生物科技有限公司 | A compound Chinese medicinal extract with antiinflammatory and antitussive effects and its application in tobacco industry |
-
1993
- 1993-04-07 CN CN93110381A patent/CN1045967C/en not_active Expired - Fee Related
Non-Patent Citations (3)
| Title |
|---|
| 《中草经成分化学》1980年7月第一版 1980. 7. 1 北京医学院,北京中医学院主编,人民卫生出版社出版 * |
| 《中草经成分化学》1980年7月第一版 1980. 7. 1 北京医学院,北京中医学院主编,人民卫生出版社出版;《时珍国药研究》1992年第3卷第4期 1992. 4. 1 胥戈;"土贝母化学成分及药理研究概况" * |
| 《时珍国药研究》1992年第3卷第4期 1992. 4. 1 胥戈;"土贝母化学成分及药理研究概况" * |
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| Publication number | Publication date |
|---|---|
| CN1093272A (en) | 1994-10-12 |
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