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Extraction and enrichment method of fritillaria total alkaloids

A total alkaloid enrichment technology, which is applied in the direction of pharmaceutical formulations, plant raw materials, medical preparations containing active ingredients, etc., can solve the problems of insufficient total alkaloid content, emulsification, low alkaloid content, etc.

Active Publication Date: 2012-09-19
BEIJING UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This document believes that from the perspective of extraction solvent, choosing chloroform, dichloromethane or ethyl acetate has no effect on the final alkaloid content, so it is preferred to use ethyl acetate with lower toxicity as the extraction solvent; in terms of extraction solvent, 95% Among ethanol, 75% ethanol and 2% hydrochloric acid, 75% ethanol is preferred. If hydrochloric acid is used as the extraction solvent, a large amount of water-soluble components in the fritillaria will be extracted, causing serious emulsification during extraction, resulting in incomplete extraction. Therefore, compared with ethanol, when hydrochloric acid is used as the extraction solvent, the extracted alkaloid content is low
[0007] However, when using the above literature method to extract the total alkaloids of Fritillaria japonicus, the total alkaloid content in the extract cannot reach more than 50% as stipulated in the "Measures for the Administration of Drug Registration"

Method used

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  • Extraction and enrichment method of fritillaria total alkaloids
  • Extraction and enrichment method of fritillaria total alkaloids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 150 g of Fritillaria herbaceae (bean size), and extract 6 times the amount (that is, use 6 mL of hydrochloric acid per 1 g of Fritillaria, the same as the 6 times the amount described below) hydrochloric acid solution with a mass fraction of 0.5% to extract twice, 1 hour each time, Concentrate the extract until each mL of concentrated solution is equivalent to 0.5-0.7 g of the original medicinal material, centrifuge the above-mentioned concentrated solution, take the supernatant and dilute it to 250 mL with water, adjust the pH to 8 with 10% NaOH solution Extract 6 times with dichloromethane of 0.5 times volume (that is, 0.5 times volume of the above-mentioned supernatant after adjusting the pH value, the 0.5 times volume described below is the same as this), collect the dichloromethane layer, and recycle wherein The resulting extract was dried with dichloromethane to obtain 189 mg of total alkaloid crude extract dry paste.

[0024] The total alkaloid crude extract...

Embodiment 2

[0026] Take 150 g of Fritillaria fritillaria medicinal material (bean size), 4 times the amount (that is, use 4 mL of hydrochloric acid per 1 g of Fritillaria, the same as the 4 times the amount described below) hydrochloric acid solution with a mass fraction of 1% and extract twice, 1 hour each time, Concentrate the extract until each mL of concentrated solution is equivalent to 0.5-0.7 g of the original medicinal material, centrifuge the above-mentioned concentrated solution, take the supernatant and dilute it to 250 mL with water, adjust the pH to 8 with 10% NaOH solution Extract with an equal volume of dichloromethane for 3 times, collect the dichloromethane layer, and recover the dichloromethane therein to dry the obtained extract to obtain 180 mg dry paste of the crude extract of total alkaloids.

[0027] The total alkaloid crude extract dry paste obtained above was dissolved in hydrochloric acid with a mass fraction of 1%, to obtain 1 g·mL of the original medicinal mater...

Embodiment 3

[0029] Take 400 g of Fritillaria fritillaria medicinal material (bean grain size), 3 times the amount (that is, use 3 mL of hydrochloric acid per 1 g of Fritillaria, the same as the 3 times the amount described below) hydrochloric acid solution with a mass fraction of 2% and extract twice, 1 hour each time, Concentrate the extract until each mL of concentrated solution is equivalent to 0.5-0.7 g of the original medicinal material, centrifuge the above-mentioned concentrated solution, take the supernatant and dilute it to 500 mL with water, and adjust the pH value to 8 with 10% NaOH solution. Extract with an equal volume of dichloromethane for 4 times, collect the dichloromethane layer, and recover the dichloromethane therein to dry the obtained extract to obtain 490 mg dry paste of the crude extract of total alkaloids.

[0030] The total alkaloid crude extract dry paste obtained above was dissolved in hydrochloric acid with a mass fraction of 2%, to obtain 1 g·mL of the origina...

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Abstract

The invention relates to an extraction and enrichment method of fritillaria total alkaloids, comprising the following steps of: first, taking fritillaria, extracting with hydrochloric acid with the mass fraction of 0.5-2%, concentrating the extracting solution, centrifuging the concentrated solution, taking the supernatant; second, regulating the pH of the supernatant to 8-11, extracting with dichloromethane, collecting the dichloromethane, recovering the solvent until dried to obtain the total alkaloid crude extract; and third, dissolving the total alkaloid crude extract with hydrochloric acid with the mass fraction of 0.5-2%, regulating the pH to 8-11, taking the loading solution, enabling the loading solution to pass through HPD100 type or HPD722 type macroporous resin columns, washingwith water until the eluent is colorless and represents negative shown by sugar detecting reaction, eluting with ethanol with the volume fraction of 90-95% until the eluent represents negative shown by alkaloid detecting reaction, collecting the ethanol eluent, and recovering the solvent until dried to obtain the total alkaloid extract. By the extraction and enrichment method of fritillaria totalalkaloids provided by the invention, the purity of the obtained fritillaria total alkaloids is high.

Description

technical field [0001] The invention relates to a method for extracting and enriching total alkaloids from Fritillaria japonicus, in particular to a method for extracting and enriching total alkaloids from Fritillaria japonicus. Background technique [0002] Fritillaria thunbergii is the dried bulb of Fritillaria thunbergii Miq., a plant of the genus Fritillaria in the family Liliaceae. Carbuncles, scrofula, and sores. The effective parts of Fritillaria are total alkaloids, including peiminine, peiminine, zhebeining, zhebeibingsu, zhebeiketone, fritillaria, peimofenine, fritilline, Fritidine base and so on. [0003] The total alkaloid content in Fritillaria fritillata is very low, only 0.12%-0.25% (mass fraction), which brings special difficulties to the extraction of total alkaloids from Fritillaria fritillata. When the method of extracting and enriching the total alkaloids of Fritillaria japonicus was used, the content of alkaloids in the total alkaloid extract of Friti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/8966A61K125/00
Inventor 韩立炜刘斌胡凯文安超唐民科董洁
Owner BEIJING UNIV OF CHINESE MEDICINE
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