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Process for preparing caulopyhllum robustum total alkali

A preparation process and technology of Radix Radix are applied in the field of preparation technology of Radix Radix et Rhizoma total alkaloids, and can solve problems such as easy generation of emulsification, unfavorable industrial production, waste and the like

Inactive Publication Date: 2005-05-18
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to use a large amount of chloroform and n-butanol, it will be extracted many times, and it is easy to produce emulsification, which is not conducive to industrial production, and it is not easy to extract completely, resulting in waste. Impurities (such as saponins)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0020] Experimental example 1: Investigation of sample loading flow rate

[0021] 2% hydrochloric acid extract (every 12.5ml extract is equivalent to 1g extract or 3g raw medicinal material) is loaded on LSD001 type cation exchange resin column (resin weighs 80g, column volume is 100ml, column diameter: column height=1:2) During the process, different flow rates were used to improve the detection of bismuth potassium iodide reagent, and the relationship between sample loading flow rate and adsorption capacity was investigated. The results are as follows:

[0022] Sample flow rate

[0023] Equivalent to the amount of raw medicinal materials

[0024] Loading volume (ml) equivalent extract volume (g)

[0025] (ml.min -1 )

[0026] (g)

[0027] 1 2200 176 528

[0028] 2 1700 136 408

[0029] 3 1300 104 312

[0030] The results showed that the flow rate of the sampl...

experiment example 2

[0031] Experimental Example 2: Investigation of Elution Solvent

[0032] The total alkaloids of Rhizoma radix that have been exchanged on the LSD001 type cation exchange resin column (resin weight 80g, column volume 100ml, column diameter: column height=1: 2) are eluted by the following systems respectively: (1) containing Methanol system with different concentrations of ammonia water; (2) Methanol system containing 2% hydrochloric acid; (3) Methanol system containing hydrochloric acid and then ammonia water; (4) Methanol system containing ammonia water and then methanol with hydrochloric acid system; with improved bismuth iodide potassium reagent detection, the elution efficiency of different elution systems was investigated, and the elution flow rate was 2ml.min -1 , the result is as follows:

[0033] Elution system (1): respectively eluted with methanol containing 2%, 5%, 10%, and 20% ammonia water. There was no significant difference in elution efficiency. It can be seen ...

Embodiment 1

[0039] Get 250g of red hair seven alcohol extract (density is about 1.32 (room temperature)), extract twice with dilute hydrochloric acid, the first time with 12 times the amount of 2% dilute hydrochloric acid, the second time with 5 times the amount of 1% dilute hydrochloric acid, Let stand and settle to obtain a total of 3100ml supernatant, take 2200ml and put it on LSD001 type cation exchange resin column. The weight of the resin is about 80g (column volume 100ml, column diameter:column height=1:2), the sample loading flow rate is 0.6 times the column volume per hour, wash the column with tap water after loading the sample, until the pH of the water eluent is 6-7, discard Remove the eluent; first elute with 8 times column volume of methanol containing 2% ammonia water, then use 4 times column volume of methanol containing 2% hydrochloric acid to elute, the flow rate of eluent should be controlled at 0.5-0.6 per hour times the column volume, during the elution process, use b...

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PUM

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Abstract

The present invention discloses the preparation process of total caulopyhllum robustum alkaloid. The preparation process includes ethanol extracting and acid solution extracting caulopyhllum robustum root and rhizome, adsorbing the acid solution extract liquid in cationic exchange resin column with sample liquid flow rate of 1.1-1.3 times column volume each hour, water washing to neutrality, elution successively with methanol containing 2-4 % ammonia water and methanol containing 1-2 % hydrochloric acid with the eluent flow rate of 0.5-0.6 times column volume each hour, merging the eluent and concentration to obtain caulopyhllum robustum extractum.

Description

technical field [0001] The invention relates to a method for extracting the total alkaloids of the seven-headed seven-headed root and the rhizome, in particular to a preparation process of the seven-headed total alkaloid. Background technique [0002] Radix et Rhizoma Leonticis (Radix et Rhizoma Leonticis) is the root and rhizome of Leonticerobustum (Maxim.) Diels., a plant of the family Berberidaceae. 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. Contains alkaloids such as Magnoline, Taspinine, N-methylcytisine, D-lupine. It has a variety of pharmacological effects such as lowering blood pressure, stimulating uterine smooth muscle, antibacterial, antiviral, anti-inflammatory, anti-rheumatic, and anti-spasmodic. It has great research value, but there are few domestic researches at present. [0003] Before this process, there was no m...

Claims

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Application Information

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IPC IPC(8): C07D221/18C07D455/00C07G5/00
Inventor 贺浪冲何强李义平李翠芹王娜陈方
Owner XI AN JIAOTONG UNIV