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Method for preparing bayogenin from bolbostemma paniculatum

A technology for becalysapogenin and fritillaria, which is applied in the field of preparation of becalysaponin, can solve the problems of large sample loss, low yield, complicated operation and the like, and achieves the effects of maintaining stability, high yield and simple process

Inactive Publication Date: 2013-02-06
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all use column chromatography, the production cycle is long, the sample loss is large, and toxic organic solvents such as chloroform are used at the same time.
There are also literatures that use multi-step reaction semi-synthesis to obtain calyxogenin, but the operation is cumbersome and the yield is low, so it is difficult to prepare calyxogenin in large quantities

Method used

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  • Method for preparing bayogenin from bolbostemma paniculatum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take the fritillaria bulbs and crush them with a pulverizer, weigh 10kg of dry powder, add 12 times the weight of methanol, soak and extract at room temperature for 20 hours, filter, repeat the above operation on the filter residue, and extract twice, combine the filtrates, and concentrate under reduced pressure to obtain an extract , to obtain the crude extract of Fritillaria; get the extract and add 2 times the amount of water to disperse, then extract 2 times with dichloromethane equal to the volume of water, combine the dichloromethane layers, and reclaim the dichloromethane under reduced pressure (for Next extraction use), continue to extract the water layer with water-saturated n-butanol for 3 times, separate the upper layer, which is the n-butanol layer, combine the n-butanol layer, and recover n-butanol under reduced pressure (for the next extraction) to obtain a total Saponins: add an appropriate amount of water to the total saponins and azeotrope for 30 minutes...

Embodiment 2

[0018] Take the fritillaria bulbs and crush them with a pulverizer, weigh 10kg of dry powder, add 20 times the weight of methanol to soak and extract at room temperature for 18 hours, filter, repeat the above operation on the filter residue, and extract 3 times, combine the filtrates, and concentrate under reduced pressure to obtain an extract , to obtain the crude extract of Fritillaria; get the extract and add 2 times the amount of water to disperse, then extract 2 times with dichloromethane equal to the volume of water, combine the dichloromethane layers, and reclaim the dichloromethane under reduced pressure (for Next extraction use), continue to extract the water layer with water-saturated n-butanol for 3 times, separate the upper layer, which is the n-butanol layer, combine the n-butanol layer, and recover n-butanol under reduced pressure (for the next extraction) to obtain a total Saponins: add an appropriate amount of water to total saponins and azeotrope for 1 hour, co...

Embodiment 3

[0020] Take the fritillaria bulbs and crush them with a pulverizer, weigh 10kg of dry powder, add 15 times the weight of methanol, soak and extract at room temperature for 12 hours, filter, repeat the above operation on the filter residue, and extract twice, combine the filtrates, and concentrate under reduced pressure to obtain an extract , to obtain the crude extract of Fritillaria; get the extract and add 2 times the amount of water to disperse, then extract 3 times with dichloromethane equal to the volume of water, combine the dichloromethane layers, and reclaim the dichloromethane under reduced pressure (for Next extraction use), continue to extract the water layer with water-saturated n-butanol for 3 times, separate the upper layer, which is the n-butanol layer, combine the n-butanol layer, and recover n-butanol under reduced pressure (for the next extraction) to obtain a total Saponins: add an appropriate amount of water to the total saponins and azeotrope for 1 hour, co...

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Abstract

The invention discloses a method for preparing bayogenin from bolbostemma paniculatum. According to the invention, a bolbostemma paniculatum crude extract is prepared from methanol solution soak extraction. The crude extract dispersed by using a small amount of water; a dichloromethane solution is used for extraction, such that a liquid layer and a dichloromethane layer are obtained; The liquid layer is extracted by using saturated n-butanol; an n-butanol layer is separated and obtained; n-butanol is subjected to reduced-pressure recovering, such that total saponin is obtained; the total saponin is dissolved in water; a pH value is regulated to 4.5-5.5; biological enzyme is added, and enzymolysis is carried out under maintained temperature for 15-24h; an enzymolysis liquid is subjected to reduced-pressure concentration and centrifugation, such that a crude product is obtained; the crude product is subjected to cyclohexane dissolving and crystallization, such that a bayogenin crude product is obtained; the bayogenin crude product is subjected to recrystallization by using dichloromethane-methanol, and is filtered, such that bayogenin with a purity higher than 90% is obtained. According to the method, operations such as column chromatography and synthesis are not needed. The process is simple, and the organic solvent can be repeatedly utilized. The energy-consumption is low, and the conditions are mild.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine chemistry, and in particular relates to a method for preparing calyxogenin from fritillary fritillaria. Background technique [0002] Bayogenin (Bayogenin) is a pentacyclic triterpenoid component, which is currently mainly isolated from Fritillaria japonicus, and its molecular formula is C 30 h 48 o 5 , the molecular weight is 488.7, and its structural formula is as follows: [0003] [0004] The dry tuber of Bolbostem paniculatum (Maxim.) Franquet, a female family of Cucurbitaceae, is also known as Bolbostemma paniculatum (Maxim.) Franquet. It was first recorded in "Compendium of Materia Medica Supplements" in Qing Dynasty. The effect of detoxification. Mainly distributed in Hebei, Henan, Shanxi, Gansu and other provinces. Saponins are the main active ingredients of Fritillaria, with relatively large content. In addition, they also contain sterols and their glycosides and ester...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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