A kind of method of purifying dihedral chloride

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...