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Method for extracting new chamaejasmine B from stellera chamaejasme. L

A new technology of wolf toxin and Ruixiang wolf toxin, applied in the direction of organic chemistry, can solve the problems of slow separation speed of silica gel, many impurities in crude products, low specificity, etc., and achieve the effects of alleviating environmental pressure, good solubility, and easy recovery.

Inactive Publication Date: 2011-05-18
苏州北商智业管理咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Yang Shunyi et al. studied and concluded in the "Extraction Process of Antibacterial Components in Chamaejasbae Rhizome Roots" that there are more antibacterial components obtained by ethanol reflux extraction, but the crude product obtained by reflux extraction has more impurities than other methods, and further separation is required; Zhou Le etc. used ethyl acetate to extract in "Studies on the Inhibitory Active Components of Chamaejasbae Rhizome", the solvent is expensive and the cost of concentration is high; Zhang Rugang et al. compared two kinds of The effect of the extraction method after polyamide adsorption, alkali extraction, acid precipitation, and solvent extraction, but the specificity is not high
Chinese patent CN1544433 "Extraction and Separation Method and Application of Neochamasin B in Daphne chamaejasme" reports a purification method of ultrasonic extraction and silica gel chromatography, the extraction solvent is complicated, and the separation speed of silica gel is relatively slow

Method used

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  • Method for extracting new chamaejasmine B from stellera chamaejasme. L

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1 kg of dry chamaejasma root, crush it into 40 meshes, add 10L90% ethanol, extract for 1 hour and then filter out the extract once, then use 10L90% ethanol for reflux extraction for 1 hour, and filter for a second extraction liquid, the two extracts were combined and then concentrated into an extract. Dissolve the extract in sodium hydroxide solution of pH 10, filter out the insoluble matter, add hydrochloric acid solution of pH 2 to the filtrate to precipitate, centrifuge and suction filter, and retain the filter cake. Disperse the filter cake in 30% ethanol, put it on the ADS-2 macroporous resin column by wet method, wash the column with 2 times column volume deionized water, and elute the flavonoid substances with 60% ethanol until the flavonoids cannot be detected in the effluent. The resulting eluate was evaporated to dryness to a solid. The solid was dissolved in acetone, concentrated to a small volume and left to stand for crystallization, repeated twice, a...

Embodiment 2

[0027] Take 1 kg of dried Chamasa chamaejas root, crush it into 40 meshes, add 12L of 95% ethanol, extract for 1.5 hours and then filter out the extract once, then use 12L of 95% ethanol for reflux extraction for 1 hour, and then extract for the second time by suction liquid, the two extracts were combined and then concentrated into an extract. Dissolve the extract in sodium hydroxide solution of pH 10, filter out the insoluble matter, add hydrochloric acid solution of pH 2 to the filtrate to precipitate, centrifuge and suction filter, and retain the filter cake. Disperse the filter cake in 30% ethanol, put it on the AB-8 macroporous resin column by wet method, wash the column with 3 times column volume deionized water, and elute the flavonoid substances with 65% ethanol until the flavonoids cannot be detected in the effluent. The resulting eluate was evaporated to dryness to a solid. Dissolving the solid in acetone, concentrating to a small volume and standing still to cryst...

Embodiment 3

[0029] Take 1 kg of dry chamaejasma root, crush it into 60 meshes, add 15L of 90% ethanol, extract for 1.5 hours and then filter the extract once, then use 15L of 90% ethanol for reflux extraction for 1.5 hours, and then extract for the second time by suction liquid, the two extracts were combined and then concentrated into an extract. Dissolve the extract in sodium hydroxide solution of pH 10, filter out the insoluble matter, add hydrochloric acid solution of pH 2 to the filtrate to precipitate, centrifuge and suction filter, and retain the filter cake. Disperse the filter cake in 30% ethanol, put it on the AB-8 macroporous resin column by wet method, wash the column with 2 times the column volume of deionized water, and elute the flavonoid substances with 70% ethanol until the flavonoids cannot be detected in the effluent, and put The resulting eluate was evaporated to dryness to a solid. The solid was dissolved in acetone, concentrated to a small volume and left to stand f...

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Abstract

The invention provides a method for extracting new chamaejasmine B from stellera chamaejasme. L, which comprises the process steps of: reflux-extraction after pulverization of stellera chamaejasme. L, alkali extraction and acid precipitation, separation with macroporous resins and crystallization. The method has the advantages of simple operation, low carbon, economy and high purity of product.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for extracting neochamasin B from Daphne chamaejasmin. Background technique: [0002] Stellera chamaejasme (Stellera Chamaejasme.L), aliased as heartbroken grass, match head flower, etc. A perennial herb with thick roots that can be used as medicine. It is highly poisonous and can dissipate stagnation, expel water, relieve pain and kill insects. It can treat water gas swelling, lymphatic tuberculosis, and bone tuberculosis. External application can cure scabies, pruritus, intractable dermatitis, kill insect flies, and eliminate maggots. Except for the western desert area, it is widely distributed in all parts of Inner Mongolia, especially the seriously degraded grasslands, which cannot be used as green fodder. Cattle and sheep may die after eating them by mistake. For a long time, it has been a harmful plant that grassland herdsmen hate. Ho...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
Inventor 张翼李法庆钱珏
Owner 苏州北商智业管理咨询有限公司
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