Method for purifying nitidine chloride

A technology of chlorinated limpet base and limpet, which is applied in the field of separation and purification, can solve problems such as unfavorable experimental operations, large environmental pollution, and unhealthy health, and achieve the effects of high efficiency, low environmental pollution, and low toxicity

Active Publication Date: 2017-12-01
GUANGDONG LUOFUSHAN SINOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of chloroform and methanol in the experimental process are toxic reagents, which pollute the environment and are not conducive to health
[0006] The name of the invention is a method for enriching the common anti-tumor components of liangmianzhen by multi-solvent ext

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of embodiment of the method for the purification of chlorinated cinnamon of the present invention, the method described in this embodiment comprises the following steps:

[0026] (1) Grind 100 g of the LMZ medicinal material, extract 3 times with 0.5% hydrochloric acid and 95% ethanol solution under reflux, the dosage is 8 times, 6 times and 4 times in turn, reflux for 2 hours each time, filter, and combine the filtrates three times , concentrated to a small volume, recovered ethanol, adjusted the pH value to 7 with NaOH solution, stood still for 12 hours, filtered, concentrated the filtrate to a small volume, precipitated with 95% ethanol for 12 hours, refrigerated at 4°C for 12 hours, filtered After filtration, the filtrate was concentrated to a small volume, precipitated with 95% ethanol for 12 hours, refrigerated at 4°C for 12 hours, filtered, the filtrate was concentrated to 20% alcohol content, and the obtained sample solution was 200ml;

[0027] (2) Mix th...

Embodiment 2

[0031] A kind of embodiment of the method for the purification of chlorinated cinnamon of the present invention, the method described in this embodiment comprises the following steps:

[0032] (1) Grind 500g of the LMZ medicinal material, extract 3 times with 1% hydrochloric acid and 80% ethanol solution under reflux, the dosage is 8 times, 6 times and 4 times in turn, reflux for 3 hours each time, filter, and combine the filtrates three times , concentrated to a small volume, recovered ethanol, adjusted the pH value to 7 with NaOH solution, stood still for 12 hours, filtered, concentrated the filtrate to a small volume, precipitated with 95% ethanol for 12 hours, refrigerated at 4°C for 12 hours, filtered After filtration, the filtrate was concentrated to a small volume, precipitated with 95% ethanol for 12 hours, refrigerated at 4°C for 12 hours, filtered, the filtrate was concentrated to 20% alcohol content, and the obtained sample liquid was 1000ml;

[0033] (2) Mix the sa...

Embodiment 3

[0037] A kind of embodiment of the method for the purification of chlorinated cinnamon of the present invention, the method described in this embodiment comprises the following steps:

[0038] (1) Grind 100 g of the LMZ medicinal material, extract 3 times with 1% hydrochloric acid methanol solution, the dosage is 8 times, 6 times, 4 times, reflux for 2 hours each time, filter, combine the filtrate three times, concentrate To a small volume, recover the ethanol, adjust the pH value to 7 with NaOH solution, let it stand for 12 hours, filter, concentrate the filtrate to a small volume, precipitate with 95% ethanol for 12 hours, refrigerate at 4°C for 12 hours, filter, Concentrate the filtrate to a small volume, precipitate with 95% ethanol for 12 hours, refrigerate at 4°C for 12 hours, filter, concentrate the filtrate to 20% alcohol content, and obtain a sample solution of 200ml;

[0039] (2) Mix the sample solution with dry activated alumina (100-200 mesh, about 25g), grind unti...

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Abstract

The invention discloses a method for purifying nitidine chloride. The method comprises the following steps: after smashing a nitidine medicinal material, reflux-extracting by using acidity alcohol solution, merging acid alcohol extracting solution, regulating the pH value by using acid-base, stewing and filtering; alcohol-precipitating, refrigerating, filtering, and concentrating to obtain the extracting solution as sample solution; uniformly mixing the sample solution and normal phase silica gel or aluminium oxide, drying by distillation, separating and purifying through the normal phase silica gel or aluminium oxide, eluting by using ethyl acetate-absolute ethyl alcohol, recycling a solvent, collecting fractions, dissolving by using methyl alcohol, merging the fractions with the high content through the TLC identification and recrystallizing, to obtain a product as the nitidine chloride; and executing the HPLC assay, wherein the transfer rate is more than 80%, and the crystallization purity is higher than 90%. The method is capable of efficiently separating and purifying the nitidine chloride, and is suitable for the large-scale production. The toxicity is small, few solvents are used, the economic value is high, the environmental pollution is small, and the purity is high.

Description

technical field [0001] The invention relates to a method for separation and purification, in particular to a method for separation and purification of epicaline chloride by using normal phase silica gel or alumina. Background technique [0002] Zanthoxylum nitidum (Roxb.) DC] is the dried root of Zanthoxylum nitidum (Roxb.) DC, which is a commonly used clinical traditional Chinese medicine and is recorded in "Chinese Pharmacopoeia". It has the effects of promoting blood circulation and removing blood stasis, promoting qi and relieving pain, dispelling wind and promoting chromium, detoxifying and reducing swelling, etc. It can be used to treat tumbling injuries, stomach pain, toothache, neuralgia, rheumatic bone pain, poisonous snake bites; external treatment of burns and scalds, etc. The main components of LMZ medicinal materials are alkaloids, accounting for about 0.7%. Among them, LMZ is one of the active ingredients of LMZ and the main active ingredient of LMZ preparation...

Claims

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Application Information

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IPC IPC(8): C07D491/056
CPCC07D491/056
Inventor 丁扬洲冯少斌张清民
Owner GUANGDONG LUOFUSHAN SINOPHARM
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