CN1354179A - Preparation process of sophoridine - Google Patents
Preparation process of sophoridine Download PDFInfo
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- CN1354179A CN1354179A CN 00133349 CN00133349A CN1354179A CN 1354179 A CN1354179 A CN 1354179A CN 00133349 CN00133349 CN 00133349 CN 00133349 A CN00133349 A CN 00133349A CN 1354179 A CN1354179 A CN 1354179A
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- sophorine
- letones
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Abstract
The preparation process of sophoridine includes the following steps: concentrating total alkali liquor with reduced pressure, in which the sopho carpine and sophocarpidine are removed; dissolving, suction or directly extracting to obtain sophoridine crude products; finally making recrystallization so as to obtain pure product sophoridine. Said technological process is suitable for industrial production. It yield rate is high, and its purity is high.
Description
The present invention relates to alkaloidal producing, especially the preparation technology of sophorine.
Sophorine (Sophoridine) is one of contained main alkaloid of leguminous plants Herba Sophorae alopecuroidis.The clinical treatment that is used for cancer patient has better curative effect.Simultaneously, it has effects such as antisepsis and anti-inflammation.As far back as the thirties, Chinese scholars just is devoted to extract various alkaloids from Herba Sophorae alopecuroidis.The Ningxia People's Press publishes the Zhong Ren mountain and compiles in " research of Herba Sophorae alopecuroidis and utilization thereof " book, the processing method of several preparation sophorines is disclosed, mainly be to utilize strong, the weak difference of various alkaloid alkalescence in the Herba Sophorae alopecuroidis, with with a kind of solvent stage extraction, combined aluminum oxide column chromatography more separablely goes out sophorine at interior different alkaloids.But these existing process method only rest in the laboratory, are difficult to reach suitability for industrialized production.
The purpose of this invention is to provide a kind of suitability for industrialized production that is suitable for, the preparation technology of sophorine yield height, sophorine that purity is high.
For achieving the above object, the present invention is by the following technical solutions:
The preparation technology of sophorine, concrete processing step is as follows:
(1) will remove total alkali lye of sophocarpine, matrine, and transfer pH value, use a kind of extraction in haloalkane, hydro carbons, benzene class, the ethers then to alkalescence, the extraction liquid concentrating under reduced pressure, again through the alcohols material dissolving, lysate gets the sophorine crude product through suction filtration, concentrating under reduced pressure behind the concentrating under reduced pressure;
(2) that the sophorine crude product is constituted separately with letones or letones and alcohols material, letones and ether material, letones and Ester mix the solvent recrystallization of formation respectively, sophorine.
The preparation technology of sophorine, concrete processing step also can be:
(1) will remove total alkali lye of sophocarpine, matrine, and transfer pH value, use a kind of extraction in haloalkane, hydro carbons, benzene class, the ethers then to alkalescence, the extraction liquid concentrating under reduced pressure, the sophorine crude product;
(2) that the sophorine crude product is constituted separately with letones or letones and alcohols material, letones and ether material, letones and Ester mix the solvent recrystallization of formation respectively, sophorine.
The present invention has following effect:
(1) processing method is simple and practical.
(2) product purity height.Calculate with dry product, products obtained therefrom content can reach more than 98%.
(3) produce sophorine yield height.
(4) save cost, various solvents can recycle.
(5) processing method is suitable for suitability for industrialized production.
The invention will be further described below in conjunction with embodiment.
Fig. 1 is a process flow sheet of the present invention.
Embodiment 1:
To remove total alkali lye of sophocarpine, matrine, and transfer pH value to alkalescence with sodium hydroxide, toluene or benzene, xylene extraction, repetitive operation, combining extraction liquid, crystallization is separated out in concentrated, cooling, and suction filtration obtains the sophorine crude product.Is 90: 10 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product with the ratio of acetone, dehydrated alcohol, and resulting crystallization is 80: 20 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 2:
To remove total alkali lye of sophocarpine, matrine, and transfer pH value to alkalescence with sodium hydroxide, chloroform extraction, repetitive operation, combining extraction liquid, crystallization is separated out in concentrated, cooling, and suction filtration obtains the sophorine crude product.Is 80: 20 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product with the ratio of acetone, dehydrated alcohol, and resulting crystallization is 70: 30 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 3:
To remove total alkali lye of sophocarpine, matrine, and transfer pH value to alkalescence with sodium hydroxide, petroleum ether extraction, repetitive operation, combining extraction liquid, crystallization is separated out in concentrated, cooling, and suction filtration obtains the sophorine crude product.S' 50: 50 mixed solvent acetone, dehydrated alcohol recrystallization 2-3 time with 20kg sophorine crude product with the ratio of acetone, dehydrated alcohol, resulting crystallization is 95: 5 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 4:
To remove total alkali lye of sophocarpine, matrine, to alkalescence, hexanaphthene extracts with sodium hydroxide accent pH value, repetitive operation, and combining extraction liquid concentrates, cools off, and separates out crystallization, and suction filtration obtains the sophorine crude product.S' 50: 50 mixed solvent acetone, dehydrated alcohol recrystallization 2-3 time with 20kg sophorine crude product with the ratio of acetone, dehydrated alcohol, resulting crystallization is 95: 5 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 5:
Producing of sophorine crude product is identical with embodiment 1,2,3,4, during recrystallization, it at first with the ratio of acetone, dehydrated alcohol 90: 10 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product, resulting crystallization is 80: 20 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 6:
Producing of sophorine crude product is identical with embodiment 1,2,3,4, during recrystallization, it at first with the ratio of acetone, dehydrated alcohol 80: 20 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product, resulting crystallization is 70: 30 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 7:
Producing of sophorine crude product is identical with embodiment 1,2,3,4, during recrystallization, it at first with the ratio of acetone, dehydrated alcohol 50: 50 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product, resulting crystallization is 50: 50 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 8:
Producing of sophorine crude product is identical with embodiment 1,2,3,4, during recrystallization, it at first with the ratio of acetone, dehydrated alcohol 50: 50 mixed solvent recrystallization 2-3 time with 20kg sophorine crude product, resulting crystallization is 50: 50 mixed solvent recrystallization 2-3 time again with the ratio of sherwood oil, acetone, promptly obtains the pure product 10kg of sophorine.
Embodiment 9:
With the total alkali lye behind the proposition matrine, be evaporated to no cut and flow out, dissolve with ethanol, suction filtration, filtrate decompression concentrates, and obtains the sophorine crude product, and the pure product of sophorine are refining, and method with embodiment 1,2,3,4,5,6,7,8 is identical respectively.
Sherwood oil, chloroform, benzene,toluene,xylene, cyclohexane give are that extract can mutual alternative in above embodiment 1,2,3,4,5,6,7,8,9.
Claims (10)
1. the preparation technology of sophorine, concrete processing step is as follows:
(1) will remove total alkali lye of sophocarpine, matrine, and transfer pH value, use a kind of extraction in haloalkane, hydro carbons, benzene class, the ethers then to alkalescence, the extraction liquid concentrating under reduced pressure, again through the alcohols material dissolving, lysate gets the sophorine crude product through suction filtration, concentrating under reduced pressure behind the concentrating under reduced pressure;
(2) that the sophorine crude product is constituted separately with letones or letones and alcohols material, letones and ether material, letones and Ester mix the solvent recrystallization of formation respectively, sophorine.
2. the preparation technology of sophorine, concrete processing step is as follows:
(1) will remove total alkali lye of sophocarpine, matrine, and transfer pH value, use a kind of extraction in haloalkane, hydro carbons, benzene class, the ethers then to alkalescence, the extraction liquid concentrating under reduced pressure, the sophorine crude product;
(3) that the sophorine crude product is constituted separately with letones or letones and alcohols material, letones and ether material, letones and Ester mix the solvent recrystallization of formation respectively, sophorine.
3. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described letones is an acetone.
4. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described alcohols material is an ethanol.
5. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described ether material is a sherwood oil.
6. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described Ester is an ethyl acetate.
7. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that in the recrystallizing technology step, in letones, the alcohols material mixed solvent, and letones 50%-95%, alcohols material 5%-50%; In letones, the ether material mixed solvent, letones 5%-50%, ether material 50%-95%; In letones, the Ester mixed solvent, letones, Ester 5%-50%, 50%-95%.
8. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described haloalkane is a chloroform.
9. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described benzene class is a benzene,toluene,xylene.
10. the preparation technology of sophorine as claimed in claim 1 or 2 is characterized in that described hydro carbons is a hexanaphthene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001333496A CN1325495C (en) | 2000-11-18 | 2000-11-18 | Preparation process of sophoridine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001333496A CN1325495C (en) | 2000-11-18 | 2000-11-18 | Preparation process of sophoridine |
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| Publication Number | Publication Date |
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| CN1354179A true CN1354179A (en) | 2002-06-19 |
| CN1325495C CN1325495C (en) | 2007-07-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB001333496A Expired - Fee Related CN1325495C (en) | 2000-11-18 | 2000-11-18 | Preparation process of sophoridine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390171C (en) * | 2004-02-10 | 2008-05-28 | 上海佳谷药业有限公司 | Method for extracting dophoridine from residual solution of matrine extracting solution from fenugreek |
| CN102550544A (en) * | 2011-11-30 | 2012-07-11 | 新疆汇通旱地龙腐植酸有限责任公司 | Dry alhagi sparsifolia alkaline essential oil and extraction and application thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1003936B (en) * | 1985-11-11 | 1989-04-19 | 和希格宝音 | Technology of comprehensively utilizing trigoella foenum-graecum l. |
| CN1052405C (en) * | 1993-01-18 | 2000-05-17 | 江西中医学院 | Anti-cancer medicine and preparation method thereof |
| JPH07188245A (en) * | 1993-12-28 | 1995-07-25 | Alps Yakuhin Kogyo Kk | New compound contained in 'kukanzo' |
| CN1044475C (en) * | 1996-09-10 | 1999-08-04 | 内蒙古苦参生化集团有限责任公司 | Preparing matrine and matrine oxide from sophora alopecuroide and its producing technology |
| CN1231890A (en) * | 1999-02-10 | 1999-10-20 | 江西中医学院 | Anticancer drug contg. diquinolizidine structure alkaloid and preparing method thereof |
-
2000
- 2000-11-18 CN CNB001333496A patent/CN1325495C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390171C (en) * | 2004-02-10 | 2008-05-28 | 上海佳谷药业有限公司 | Method for extracting dophoridine from residual solution of matrine extracting solution from fenugreek |
| CN102550544A (en) * | 2011-11-30 | 2012-07-11 | 新疆汇通旱地龙腐植酸有限责任公司 | Dry alhagi sparsifolia alkaline essential oil and extraction and application thereof |
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| CN1325495C (en) | 2007-07-11 |
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Granted publication date: 20070711 Termination date: 20121118 |