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Method for separating purified nitidine chloride by using cation exchange resin

A kind of chlorinated acanthine and cation exchange technology, which is applied in the direction of organic chemistry, can solve the problems of unhealthy producers, large environmental pollution of chloroform, etc., and achieve the effect of saving organic solvent, easy operation and high desorption rate

Inactive Publication Date: 2010-07-07
GUANGXI MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chloroform is usually used to extract the acidic aqueous solution of limpet extract, and the chloroform is recovered, and after multi-step purification, chlorinated limpet alkali can be obtained. This method of chloroform is more polluting to the environment and is also harmful to the health of producers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 300g LMZ medicinal material was pulverized, extracted 3 times with 50% ethanol solution, and the dosage was respectively 6 times, 5 times and 4 times (the volume-to-weight ratio of 50% ethanol solution to LMZ medicinal material), and the reflux extraction time 2.0h, 1.5h and 1.5h respectively in turn. After the reflux is completed, filter and combine the filtrates three times to obtain a raw material solution with a pH of 6.8.

[0025] Add the sample solution with 50% ethanol volume fraction and 140 μg / mL dihedral chloride concentration to the reagent bottle with resin, the volume ratio of ion resin and sample solution is 1:300, shake the adsorption at room temperature After 24 hours, filter, wash the resin until the washing liquid is colorless, pack the column, then desorb with 5% HCl 90% ethanol solution, first add 1BV for repeated desorption until yellow crystals can be seen, put the resin into the reagent bottle, Add the eluent several times for desorption until no ...

Embodiment 2

[0027] 300g of LMZ medicinal material was pulverized, extracted 3 times with methanol solution, the dosages were 6 times, 5 times and 4 times (volume-to-weight ratio of methanol to LMZ), and the reflux extraction time was 2.0 h, After 1.5h and 1.5h, after the reflux, filter and combine the filtrates for three times, adjust the pH of the sample solution to 3.2 with acid, and filter out the insoluble matter to obtain the sample solution, in which the concentration of dihedral chloride is 180 μg / mL.

[0028] Add the sample solution to the reagent bottle with the resin, the volume ratio of the ion resin and the sample solution is 1:400, shake the shaker at room temperature and absorb for 24 hours, filter, wash the resin until the washing solution is colorless, pack the column, and then 15 % HAC 80% ethanol solution for desorption, 1BV for repeated desorption until yellow crystals can be seen, put the resin into the reagent bottle, add eluent for desorption until no crystals are pre...

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Abstract

The invention discloses a method for separating purified nitidine chloride by using a cation exchange resin, which comprises the following steps of: (1) mixing crushed shinyleaf pricklyash root decoction pieces and a solvent for backflow extraction; and (2) regulating the pH value of sample liquid by using acid-base after the extract is filtered, performing the dynamic or static adsorption on the extract by using the cation exchange resin which has a special adsorbability for the nitidine chloride, performing desorption by using an organic acid or mixed liquid of an inorganic acid and an organic solvent, and centrifuging the stripping liquid to obtain the deposit of the nitidine chloride, wherein the resin after the desorption can be reused after being washed by a desorbing agent. The method can rapidly and efficiently separating the nitidine chloride and effectively reduce the cost and environmental pollution; and the transfer rate of the nitidine chloride is over 85 percent; and the crystalline purity is greater than 90 percent.

Description

technical field [0001] The invention relates to a cation exchange resin separation method, in particular to a cation exchange resin separation and purification method for dihedral chloride. Background technique [0002] Zanthoxylum nitidum (Roxb.) DC.] is a vine of the Rutaceae Zanthoxylum genus, which is used to treat stomach pain, toothache, neuralgia, rheumatic bone pain, snake bites and other diseases. The roots and stems of LMZ are rich in a variety of active ingredients, the main components are alkaloids, accounting for about 0.7%, and mainly benzophenanthridine alkaloids, of which LMZ chloride is the main active ingredient of LMZ preparations. It has anti-tumor, cardiotonic, blood-lowering, anti-fungal effects, especially anti-tumor activity, which has research value and development and utilization prospects. Therefore, it is of great significance to separate and purify the chlorinated double-sided needles. [0003] At present, most of the researches on the chlorina...

Claims

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Application Information

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IPC IPC(8): C07D491/056
Inventor 龙盛京卢凌春
Owner GUANGXI MEDICAL UNIVERSITY
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