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Method for extracting radix gaulophylli total alkaloid in radix gaulophylli extract liquid

A technology of total alkaloids, Rhizoma Rhizoma, applied in the direction of sugar derivatives, sugar derivatives, drug combinations, etc., can solve the problems of ion resin being easily broken, affecting the safety of preparations, increasing process steps, etc., and achieving high alkaloid transfer rate. , No resin monomer residue, 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 avoids the use of a large amount of organic solvents, and has a certain degree of progress, but there are still serious defects: in the test, it can be found that although the method can improve the purity of alkaloids, the use of methanol will bring Residues of resin monomer components such as styrene and divinylbenzene affect the safety of preparations; in the method, ammoniacal methanol and acidic methanol are used for elution in sequence, which will lead to a strong acid-base reaction, and the ion resin is easily broken and cannot be reused , which increases the production cost; at the same time, due to the use of methanol elution in the process, it is also required to increase the methanol treatment step in the pre-treatment of the resin, and the methanol 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 Rhododendron chinensis, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust pH=3, centrifuge, and the supernatant is passed through cation exchange at 4 times the column volume / hour Resin (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, and the eluate was collected until The alkaloid 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 the total alkaloids of Trichosanthes chinensis.

Embodiment 2

[0036] Get 1000g of Rhododendron 1000g, add pH=5 acidic water for percolation, combine the percolation liquid and add water to dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (Doulex 50, sodium type, diameter-to-height ratio 1:5), wash with water until the effluent is colorless, then elute with 5% hydrochloric acid solution, the elution rate is 4 times the column volume / hour, after elution is 2 times the column volume, soak for 5 hours , and then eluted until the alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), the acid eluate was collected, neutralized to neutral with calcium hydroxide, desalinated, the filtrate was concentrated and dried to obtain the red hair seven total alkaloids.

Embodiment 3

[0038] Take 5 kg of Rhododendron chinensis, add 70% ethanol for ultrasonic extraction twice, add 5 times the amount each time, ultrasonicate for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH = 2, centrifuge, and remove the supernatant with 2 times the 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 wash with 1% hydrochloric acid solution (containing 1% sodium chloride) Elute, the elution rate is 5 times the column volume / hour, collect the eluate until the alkaloid test is negative (the effluent is added dropwise with 10% silicotungstic acid without precipitation), neutralize to neutral with sodium hydroxide, and desalt , the filtrate was concentrated and dried to obtain the total alkaloids of Rhizoma radix.

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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 an extracting solution of the traditional Chinese medicine, namely root of blue cohosh, and belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal: taking the extracting solution of the root of blue cohosh; adjusting the pH value of the extracting solution to between 1 and 7; filtering the extracting solution; taking and adding the filtrate to a cation exchange resin column; rinsing the filtrate and removing the impurities; eluting the filtrate with 0.5 to 15 percent acid liquor; collecting eluent; adding alkali to the eluent for neutralization; performing desalting treatment on the mixed solution; and obtaining the root of blue cohosh total alkaloid. The method overcomes the defects of low extracting rate, large using level of organic solvent, complicated process, inability of large-scale production, and the like in the prior art and can efficiently separate high purity of the root of blue cohosh total alkaloid from the extracting solution of the root of blue cohosh.

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 alkaloids of the seven-headed seven-headed extract from the extract of the seven-headed Chinese medicine, and belongs 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. Radix et Rhizoma Leonticis is the root and rhizome of Leontice robustum (Maxim.) Diels., a small cluster plant. It is produced in the Qinling Mountains and Daba Mountains. It is also distributed in the former Soviet Union and Japan. It is a natural medicine that is not included in the Pharmacopoeia. , has the effect of regulating qi and relieving pain, expelling wind and activating bl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/29A61P15/00A61P31/04A61P29/00A61P31/12C07H5/00A61K125/00
Inventor 刘英辉李蓉朴美善
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV