Preparation method of plumbagin

A technique of plumbagin and leaching method, applied in the field of preparation of plumbagin, can solve the problems of low purity, inability to meet the needs of research and future market demands, and low extraction rate, and achieves high extraction purity and equipment. The effect of low requirements and large adsorption capacity

Inactive Publication Date: 2011-02-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have low extraction rates and low purity, which cannot meet the needs of research and future market demands.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 2 kilograms of Plumbago, artificially chopped into raw materials of 1mm, put into the still, add deionized water in the still, the addition is 2 times of the raw material by weight, the extraction time is 10 hours, and the oil and water are separated to obtain Plumbagin crude product 32g, dissolve crude product with a small amount of ethanol, go up macroporous adsorption resin column D101, 2 times of column volume deionized water elute impurity, then use sherwood oil-acetone (20:1), sherwood oil-acetone ( 10:1) and acetone-methanol (1:1) for 3 times column volume elution, collect the target eluent under the guidance of thin layer chromatography and recover the solvent, concentrate and dry, add 70% ethanol to heat and reflux to saturate and dissolve, cool , deionized water was slowly added dropwise, left to stand for crystallization, and dried to obtain 6 g of the product with a content of 96%. Check with a silica gel plate, wherein the silica gel plate is made of CMC-Na...

Embodiment 2

[0024] 2 kilograms of Plumbago, pulverized into a raw material product of 1 mm with a tissue pulverizer, put into the still, add deionized water in the still, the amount added is 2.5 times of the amount of raw material by weight, the extraction time is 8 hours, and the oil and water are separated , obtain plumbagin crude product 28g, dissolve crude product with a small amount of ethanol, go up macroporous adsorption resin column D101, 2 times column volume deionized water elutes impurity, then respectively use petroleum ether-acetone (10:1), petroleum ether- Acetone (5:1) and acetone-methanol (1:3) were eluted with 3 times the column volume each. Under the guidance of thin layer chromatography, the target eluent was collected and the solvent was recovered, concentrated to dryness, and heated to reflux with 80% ethanol to saturate and dissolve , cooled, slowly added deionized water dropwise, left to stand for crystallization, and dried to obtain 5.3g of product with a content of...

Embodiment 3

[0026] Plumbago 2 kg, crushed into a 1mm raw material with a tissue grinder, put into a multifunctional extraction tank, add 4 times the amount of chloroform solution, soak at room temperature, extract for at least 12 hours, repeatedly extract 4 times, filter, and combine the filtrate After vacuum concentration and drying, apply the macroporous adsorption resin column AB-8, 1.5 times the column volume deionized water to elute impurities, and then use petroleum ether-acetone (10:1), petroleum ether-acetone (9:4), acetone -Methanol (1:2) was eluted with 3 times the column volume, collected the target eluate under the guidance of thin layer chromatography and recovered the solvent, concentrated and dried, added 75% ethanol and heated under reflux to saturate and dissolve, cooled, and slowly added deionized water, standing still for crystallization, and drying to obtain 6.4 g of the product with a content of 96%. Check with a silica gel plate, wherein the silica gel plate is made ...

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Abstract

The invention discloses a preparation method of plumbagin, which comprises the following steps of: (1) crushing a plumbago zeylanica medicinal material into a 0.5-1mm raw material for later use; (2) extracting the raw material by adopting a vapor distillation method or an organic-solvent leaching method; (3) enriching and purifying vacuum-condensed and dried extract through macroporous resin, and eluting with petroleum ether-acetone and acetone-methanol; and (4) concentrating and drying an eluant, heating, reflowing, saturating and dissolving with 50-80 percent of ethanol, cooling, slowly and dropwise adding deionized water, settling for crystallization, filtering and drying to obtain the product. The method adopts a traditional crushing method and conventional equipment, has low cost and simple structure, can be used for obtaining the high-content plumbagin and supplies high-quality monomers or raw materials for the further deep research and development of plumbago zeylanica.

Description

Technical field: [0001] The present invention relates to a preparation method of plumbagin, in particular to a method for preparing plumbagin by steam distillation or solvent extraction combined with macroporous resin and recrystallization technology. Background technique: [0002] Plumbago zeylanica L. is the whole plant or root of Plumbago zeylanica L. in the Plumbago family Plumbago genus. The property of medicine is pungent, bitter, astringent, warm and poisonous. It has the effects of expelling wind and removing dampness, promoting qi and blood circulation, detoxifying and reducing swelling. Cure mainly rheumatic arthralgia, blood stasis, amenorrhea, bruises, carbuncle, scrofula, scabies and itching, snake bites. Born in areas with hot climates, it is common in damp ditchsides or open fields beside village roads. Produced in Fujian, Taiwan, Guangdong, Guangxi, Sichuan, Guizhou, Yunnan and other places. Baihuadan is mostly used as a national medicinal material. The l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/32C07C46/10
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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