Method for extracting and separating total alkaloids in prickly ash

A technology of total alkaloids and double-sided needles, which is applied in the field of extraction and separation of total alkaloids of double-sided needles, can solve the problems of increased adsorption efficiency, large environmental pollution, and high resin prices, achieving high adsorption rates, improving extraction rates, and saving energy costs Effect

Inactive Publication Date: 2009-02-11
GUANGXI MEDICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The separation of total alkaloids of L. chinensis initially used chloroform extraction method, but this method requires a large amount of chloroform, which is highly toxic and pollutes the environment; some studies believe that the separation effect is better with XDA-5 resin, but the price of the resin is high and the adsorption efficiency is high. Still needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Accurately weigh 2Kg of Liangmianzhen medicinal material granules, add 12L 60% (v / v) ethanol-0.5wt% inorganic acid, reflux in a water bath at 93-95°C for 1 hour, and filter; add 10L 60% (v / v) ethanol- Reflux 0.5wt% mineral acid for 0.5h, filter; add 8L of 60% (v / v) ethanol-0.5wt% mineral acid to the residue, reflux for 0.5h, filter, combine the two filtrates, recover ethanol under reduced pressure until there is no alcohol smell , stand overnight, take the supernatant, the precipitate is repeatedly kneaded and dissolved with 0.5wt% mineral acid, filtered, and combined with the supernatant. Put the extract on a macroporous resin column, elute with acid water first, then elute with 70% (v / v) ethanol, collect the 70% (v / v) ethanol eluate, recover ethanol, dry to obtain the total alkaloids The crude product has a yield of 93.6%, a total alkaloid content of more than 25%, and a total alkaloid extraction rate of 93.5%.

Embodiment 2

[0021] Accurately weigh 10.00g of LMZ powder, add 60mL of 60% (v / v) ethanol-0.5wt% mineral acid, soak for 24 hours at room temperature, filter, squeeze dry; add 60mL of 60% (v / v) ethanol-0.5 Impregnate wt% mineral acid at room temperature for 24h, filter and squeeze dry; add 60mL of 60% (v / v) ethanol-0.5wt% mineral acid to the residue and soak for 24h at room temperature, filter, squeeze dry, combine the filtrate, and filtrate is reduced Press to recover ethanol until there is no alcohol smell, let it stand overnight, take the supernatant, stir and dissolve the precipitate with 0.5wt% inorganic acid repeatedly, filter, combine the filtrate and supernatant, put it on a macroporous resin column, and first elute with acid water , then eluted with 60% (v / v) ethanol, collected 60% (v / v) ethanol eluate, reclaimed ethanol, dried to obtain the crude product of total alkaloids, the yield was 92.5%, and the total alkaloid content reached 27 %above. The total alkaloid extraction rate is...

Embodiment 3

[0023] Accurately weigh 10.00g of Liangmianzhen medicinal powder, add 50mL 60% (v / v) ethanol-0.5wt% inorganic acid to infiltrate at room temperature for 24 hours, slowly add 450mL 60% (v / v) ethanol-0.5wt% inorganic acid At the same time, percolate at a speed of 1mL / min, filter, and squeeze dry. The filtrate is decompressed to recover ethanol until it has no alcohol smell, and stands overnight. Take the supernatant, and the precipitate is dissolved by repeated stirring with 0.5wt% inorganic acid, and filtered. , the filtrate is combined with the supernatant, and the macroporous resin column is used for elution with acid water, then elution with 50% (v / v) ethanol, collecting 50% (v / v) ethanol eluate, reclaiming ethanol, Drying, the total alkaloid crude product is obtained, the yield is 91.8%, and the total alkaloid content reaches more than 27%. The total alkaloid extraction rate is 73.5%.

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Abstract

The invention discloses a method for extracting and separating the total alkaloids of shiny leaf pricklyash root; the method comprises the following steps: the shiny leaf pricklyash root is crushed, extracted for 1 time to 5 times with acid water-alcohol as a solvent and filtered; the filtrates are combined and decompressed, have the solution removed so that no alcoholic odor exists and are set stewing and delaminated; the supernatant fluid is fetched, and the sediment is repeatedly dissolved by acid water and filtered to obtain a filtrate which is combined with the supernatant fluid, adsorbed by a macroporous resin column and washed by an organic solvent, and then the solvent is recovered to obtain a crude alkaloid product. The method of the invention increases the extraction ratio to more than 93 percent by adding acid for extraction, and macroporous resin is used for separating alkaloids, simple and easy operated, achieving a yield rate about 93 percent.

Description

technical field [0001] The invention relates to a method for extracting and separating traditional Chinese medicinal materials, in particular to a method for extracting and separating total alkaloids of liangmianzhen. Background technique [0002] The existing method for extracting the total alkaloids of LMZ is reflux extraction with methanol, 60% ethanol or 95% ethanol. Methanol is highly toxic and is generally used for continuous reflux extraction, which is not suitable for industrial production; 95% ethanol reflux extraction is a method used by early researchers to study chemical components and their pharmacological activities, and the extraction rate of total alkaloids is relatively low. It is not suitable for industrial production; take a Ding-shaped double-sided needle medicinal material about 1 cubic centimeter in size and reflux twice with 60% ethanol, the first 9 times the amount of reflux for 2 hours, the second time 7 times the amount of reflux for 1.5 hours, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/758
Inventor 龙盛京陆世惠
Owner GUANGXI MEDICAL UNIVERSITY
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