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Method for separating ergot total alkaloids in ergot stem extract

A technology of total alkaloids and extracts, applied in the direction of alkaloids, alkaloids, drug combinations, etc., can solve the problems of difficult implementation, cumbersome operation, low transfer rate, etc., and reduce the process of regeneration resin column and alkaloid transfer rate High, simple process effect

Inactive Publication Date: 2009-07-29
BEIJING HERUN INNOVATION PHARMA TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can improve the purity of alkaloids, which has a certain degree of progress, but there are still serious defects: in the test, it can be found that due to the use of alkalinized resins such as ammonia water, the total alkaloids are not completely free, and the Soxhlet extraction method is not completely extracted. , the transfer rate is not high; free ergot total alkaloids under alkaline conditions need to have good solubility in organic solvents, but the use of organic solvents will bring resin monomer components styrene, Residues such as divinylbenzene affect the safety of the preparation; in the test, the resin needs to be poured out and transferred to a Soxhlet extractor for extraction, which is cumbersome and difficult to implement in large-scale production; at the same time, due to the use of organic solvents in the process, it is also required Ethanol treatment steps must be added to the treatment, and ethanol must be recovered later, which increases the process steps and increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 1000g of ergot decoction pieces, decoct twice with water, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust pH=3, centrifuge, and the supernatant passes through the cation exchange resin at 4 times the column volume / hour (001×7, hydrogen type, diameter-to-height ratio 1:8), washed with water until the effluent was colorless, then eluted with 15% hydrochloric acid solution, the elution rate was 2 times the column volume / hour, collected the eluate, and sent to biological The alkali test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain total ergot alkaloids.

Embodiment 2

[0036] Get 1000g of ergot decoction pieces, add the acidic water of pH=5 to percolate, combine the percolate and add water and dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (Doulex 50 with 5 times column volume / hour) , sodium type, diameter-to-height ratio 1:5), washed with water until the effluent was colorless, then eluted with 5% hydrochloric acid solution, the elution rate was 4 times the column volume / hour, soaked for 5 hours after elution was 2 times the column volume, Then elute until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), collect the acid eluate, neutralize it with calcium hydroxide, remove salt, concentrate and dry the filtrate to obtain the total alkaloids of ergot .

Embodiment 3

[0038] Take 5 kg of ergot decoction pieces, add 70% ethanol to ultrasonically extract twice, add 5 times the amount each time, ultrasonically for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH = 2, centrifuge, supernatant with 2 Times column volume / hour Pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), wash with water until the effluent is colorless, and then elute with 1% hydrochloric acid solution (containing 1% sodium chloride) , the elution rate is 5 times column volume / hour, collect the eluate until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), neutralize to neutral with sodium hydroxide, desalt, The filtrate was concentrated and dried to obtain the total alkaloids of ergot.

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Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating total alkaloid from traditional Chinese medicine ergot extract, which belongs to the field of traditional Chinese medicine. The method comprises the following technical proposal that the ergot extract is taken and filtered after the pH value of the ergot extract is adjusted to be between 1 and 7; filtrate is added to a cation exchange resin column, eluted with water to remove impurities and then eluted by use of 0.5 to 15 percent acid liquid; and eluent is collected, added with alkali for neutralization and desalted so as to prepare ergot total alkaloid. The method overcomes the deficiency that the prior art is low in extraction ratio, large in the amount of organic solvents, complex in process, incapable of mass production and the like, and can efficiently separate high-purity ergot total alkaloid from the ergot extract.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating total ergot alkaloids from traditional Chinese medicine ergot extracts, belonging to the field of traditional Chinese medicines. Background technique [0002] Alkaloids are a large class of basic nitrogen-containing compounds that widely exist in nature, are active ingredients of many Chinese herbal medicines, and are an important class of substances in nature. The ergot taste is slightly bitter, flat and poisonous. It is the sclerotium formed by the ergot fungus Clavicepspurpurea (Fr.) Tulasne (Secales cornutum) parasitizing in the ovary of the gramineous plant rye Secale cereale. It is a commonly used Folk Chinese herbal medicine has the effects of stopping bleeding, regulating menstruation, and relieving headaches. Studies have shown that total ergot alkaloids are its main effec...

Claims

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Application Information

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IPC IPC(8): A61K36/899A61P7/04A61P15/00A61P25/04C07G5/00
Inventor 刘英辉武建卓王广录
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV