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Method for separating and purifying peimisine from fritillaria by using high-speed countercurrent chromatography

A high-speed countercurrent chromatography, separation and purification technology, applied in the field of high-speed countercurrent chromatography (HSCCC) to separate and purify fritillary from fritillary, can solve the problems of large consumption of organic reagents, long separation period, low recovery efficiency, etc. Short preparation time, less sample loss, and simple operation

Inactive Publication Date: 2014-05-07
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the existing methods for separating and purifying fritillaria from fritillaria are mainly column chromatography, but the separation cycle is long, the operation is cumbersome, the consumption of organic reagents is large, and the recovery efficiency is low

Method used

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  • Method for separating and purifying peimisine from fritillaria by using high-speed countercurrent chromatography
  • Method for separating and purifying peimisine from fritillaria by using high-speed countercurrent chromatography
  • Method for separating and purifying peimisine from fritillaria by using high-speed countercurrent chromatography

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Embodiment 1

[0020] A method for separating and purifying fritillaria from fritillaria by high-speed countercurrent chromatography, comprising the following steps:

[0021] (1) Preparation of crude extract of total alkaloids from Taibai Fritillaria

[0022] Take 100g of Taibai Fritillaria, crush it into a coarse powder, add ammonia water to make sure that the medicinal materials have just been submerged, alkalize for 1 hour, heat reflux with 700mL of 95% ethanol for 4 times, each time for 1.5 hours, combine the extracts from 4 times, and concentrate under reduced pressure Get the extract. Dissolve the extract with 50mL of 0.1M hydrochloric acid, filter the acid solution, extract and degrease the acid solution with petroleum ether, then use 10% sodium hydroxide to adjust the pH to 9~10, and then extract it with dichloromethane four times. The amount of methane was 100mL, 100mL, 80mL, 60mL in turn, the dichloromethane layers were combined, concentrated and dried under reduced pressure to ob...

Embodiment 2

[0031] A method for separating and purifying fritillaria from fritillaria by high-speed countercurrent chromatography, comprising the following steps:

[0032] (1) Preparation of crude extract of total alkaloids from Fritillaria wabu

[0033] Take 100 g of dried and pulverized Fritillaria wabu coarse powder (passed through a 20-mesh sieve), and prepare total alkaloids according to the method in Example 1 to obtain 578 mg of total alkaloid powder.

[0034] (2) High-speed countercurrent chromatographic separation

[0035] The application of high-speed countercurrent chromatography TBE-300B (Shanghai Tongtian Biotechnology Co., Ltd.) separation and purification fritillaria.

[0036] The two-phase solvent system for high-speed countercurrent chromatography is n-hexane-ethyl acetate-methanol-water (3:5:3:5, v / v / v). Take 50 mg of the total alkaloid powder of fritillaria obtained in step 1 and dissolve it in 6 mL of the same amount of upper phase and lower phase, and inject the sam...

Embodiment 3

[0038] Choose a solvent system with a suitable partition coefficient. It is generally believed that the partition coefficient K value between 0.5 and 2 is better for separation.

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Abstract

The invention discloses a method for separating and purifying peimisine from fritillaria by using a high-speed countercurrent chromatography. The method comprises the steps: (1) preparing total alkaloid of fritillaria by using dry fritillaria bulbs; (2) separating and purifying peimisine by using high-speed countercurrent chromatography; with a mixed solution as a stationary phase (an upper layer) and a mobile phase (a lower layer), dissolving the total alkaloid powder of the fritillaria into the equivalent mobile phase and stationary phase, introducing a sample through an injection valve, observing a chromatogram, collecting fractions when a target peak appears, and volatizing a solvent to obtain the peimisine, wherein the mixed solution is prepared from n-hexane, ethyl acetate, methyl alcohol and water according to the volume ratio of (2-4):5:(2-3):5. The method is free of solid-phase carriers and irreversible adsorption, simple, rapid, efficient and high in purity of the obtained target compound.

Description

technical field [0001] The invention belongs to the technical field of natural medicinal chemistry, and relates to a method for preparing fritillaria from traditional Chinese medicine fritillaria, in particular to a method for separating and purifying fritillaria from fritillary by using high-speed countercurrent chromatography (HSCCC). Background technique [0002] The isosteroid alkaloid cyclopamine (cyclopamine) found in Liliaceae Fritillaria, Veratrum and other plants is one of the most concerned anti-tumor natural products in the world. Studies have shown that it is a A Hedgehog pathway inhibitor, which has good inhibitory effects in vivo and in vitro on various cancers such as non-small cell lung cancer, gastric cancer, and pancreatic cancer. Since the content of cyclopamine in plants is low and the total chemical synthesis is very difficult, it is a feasible strategy to isolate cyclopamine analogues from plants and obtain cyclopamine through semi-synthesis. At presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J43/00
Inventor 姜艳李会军戴静喻悦
Owner NANJING FORESTRY UNIV
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