CN1093272A - The preparation method of tubeimoside first element - Google Patents
The preparation method of tubeimoside first element Download PDFInfo
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- CN1093272A CN1093272A CN 93110381 CN93110381A CN1093272A CN 1093272 A CN1093272 A CN 1093272A CN 93110381 CN93110381 CN 93110381 CN 93110381 A CN93110381 A CN 93110381A CN 1093272 A CN1093272 A CN 1093272A
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- tubeimoside
- rhizoma
- bolbostemmatis
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Abstract
The Chinese crude drug Rhizoma Bolbostematis, water saturated C is used in pulverizing, rare pure lixiviate, concentrated, water dilution
4～C
5The aliphatic alcohol extraction boils off solvent, gets Rhizoma Bolbostemmatis total saponins, dissolve with methanol, and mixed solvent precipitates, and gets the plain crude product of tubeimoside first, or total Saponin hot water dissolving, macroporous adsorption resin chromatography, rare pure eluting, mixed solvent precipitates, and gets tubeimoside first element crude product.Through aqueous methanol---mixed solvent method is refining.Solvent is inexpensive, be easy to get, and toxicity is less; Technology is easy, and equipment is simple, and cost is low, is fit to national conditions, can drop into suitability for industrialized 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 Bulbus Fritillariae Uninbracteatae.
Cucurbitaceous plant Rhizoma Bolbostematis (Bolbostemma paniculatum(Maxim.) Franquet), the property hardship is slightly cold.The function eliminating stagnation, detumescence, detoxifcation.The traditional Chinese medical science is used for the treatment of acute mastitis scrofula, mastitis, lymphoid tuberculosis, chronic lymphadenitis, hypertrophic rhinitis etc.
From the Rhizoma Bolbostemmatis total saponins 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 antiinflammatory, 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 Rhizoma Bolbostemmatis total saponins after n-butanol extracting liquid concentrating under reduced pressure and the placement.Separate Rhizoma Bolbostemmatis total saponins with the silica gel H low pressure column chromatography then, obtain tubeimoside first element.
The deficiencies in the prior art are the chloroform give extractants that need with severe toxicity, separate with chromatograph of liquid, and the little cost of output is high, and process conditions 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 Rhizoma Bolbostemmatis total saponins, 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 methanol, and surplus liquid is concentrated into extractum, after 2～4 times of water gagings dilutions, uses water saturated C
4～C
5Aliphatic alcohol extraction 2～4 times, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins,
3. Rhizoma Bolbostemmatis total saponins dissolve with methanol, the mixed solvent precipitation, the plain crude product of tubeimoside first,
4. or the Rhizoma Bolbostemmatis total saponins hot water dissolving, macroporous adsorption resin chromatography, rare pure eluting, 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 Rhizoma Bolbostemmatis total saponins, adds acetone, ether or the acetone-ether mixed liquor 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
101, D
520, model such as AB-8, NKA-II macroporous adsorption resin chromatography.
The preparation method of above-mentioned tubeimoside first element, described rare pure eluting are meant earlier the ethanol flush away impurity with 25～35%, the ethanol elution tubeimoside first element of reuse 40～70%.
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, method of the present invention has following advantage:
Solvent inexpensive, 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]
Rhizoma Bolbostematis medical 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 extractum, after the dilution of 2 times of water gagings, is the water saturated n-butanol extraction 2 times of 6L with total amount, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins 0.13kg.
Above-mentioned amount Rhizoma Bolbostemmatis total saponins, use the 0.26L dissolve with methanol, in the methanol solution of Rhizoma Bolbostemmatis total saponins, add the acetone precipitation of 2 times of amounts, leave standstill 24h, get the plain crude product 0.046kg of tubeimoside first, make with extra care through the aqueous methanol dissolving-acetone method that settles out, 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%, mp251～252 ℃.
[embodiment two] Rhizoma Bolbostematis medical material 5kg is crushed to 20 orders, with 80% ethanol in 60 ℃ of lixiviates 4 times, boil off solvent, surplus liquid is concentrated into extractum, after 4 times of water gaging dilutions, with the water saturated isoamyl alcohol extraction of 20L 4 times, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins 0.125kg.
The Rhizoma Bolbostemmatis total saponins 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%, mp249～251 ℃.
[embodiment three]
Rhizoma Bolbostematis medical material 5kg, pulverized 10 mesh sieves, with 60% methanol of total amount 20L in 80 ℃ of lixiviates 2 times, boil off solvent, surplus liquid is concentrated into extractum, after 2 times of water gaging dilutions, uses the water saturated isobutanol of 5L to extract 2 times, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins 0.126kg.
Above-mentioned amount Rhizoma Bolbostemmatis total saponins, dissolve with methanol with 0.26L, in the methanol solution of Rhizoma Bolbostemmatis total saponins, add the acetone precipitation of 2 times of amounts, leave standstill 24h, get the plain crude product 0.047kg of tubeimoside first, make with extra care through the aqueous methanol dissolving-acetone method that settles out, 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] Rhizoma Bolbostematis medical material 5kg is crushed to 20 orders, uses 20L80% methanol in 60 ℃ of lixiviates 4 times, boil off solvent, surplus liquid is concentrated into extractum, extracts 4 times with the water saturated amylalcohol of 5L with 4 times of water gaging dilution backs, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins 0.131kg.
The Rhizoma Bolbostemmatis total saponins 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, get the plain crude product 0.038kg of tubeimoside first, make with extra care, leave standstill 24h through aqueous methanol dissolving-acetone, the ether mixed solvent method that settles out, 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 (5)
1, a kind of vegetable drug that belongs to 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:
1.1. at first extract Rhizoma Bolbostemmatis total saponins, secondly separate preparation tubeimoside first element,
1.2. pulverizing medicinal materials to 5～20 orders in≤80 ℃ of lixiviates 2～4 times, boils off solvent with 60～80% ethanol or methanol, surplus liquid is concentrated into extractum, after 2～4 times of water gagings dilutions, uses water saturated C
4～C
5Aliphatic alcohol extraction 2～4 times, extract pressure reducing and steaming organic solvent, vacuum drying gets Rhizoma Bolbostemmatis total saponins,
1.3. the Rhizoma Bolbostemmatis total saponins dissolve with methanol, the mixed solvent precipitation gets the plain crude product of tubeimoside first,
1.4. or the Rhizoma Bolbostemmatis total saponins hot water dissolving, macroporous adsorption resin chromatography, rare pure eluting, mixed solvent precipitation, the plain crude product of tubeimoside first.
2, according to the preparation method of the described tubeimoside first of claim 1 element, its qualifying part is described mixed solvent method precipitation, is to point in the methanol solution of Rhizoma Bolbostemmatis total saponins, adds acetone, ether or the acetone-ether mixed liquor of 2～6 times of amounts.
3, according to the preparation method of the described tubeimoside first of claim 1 element, its qualifying part is described macroporous adsorption resin chromatography, is meant to use D
101, D
520, model such as AB-8, NKA-II macroporous adsorption resin chromatography.
4, according to the preparation method of the described tubeimoside first of claim 1 element, its qualifying part is that described rare pure eluting is meant earlier the ethanol flush away impurity with 25～35%, the ethanol elution tubeimoside first element of reuse 40～70%.
5, according to the preparation method of the described tubeimoside first of claim 1 element, its qualifying part is that the plain crude product of described tubeimoside first is refining through the method that aqueous methanol dissolving-mixed solvent settles out.
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 true CN1093272A (en) | 1994-10-12 |
| CN1045967C 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) |
Cited By (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 |
| CN111233963A (en) * | 2020-03-02 | 2020-06-05 | 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
Cited By (7)
| 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 |
| CN111233963A (en) * | 2020-03-02 | 2020-06-05 | 河南中医药大学 | Active monomer for treating esophageal cancer, and composition and application thereof |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1045967C (en) | 1999-10-27 |
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