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Method for extracting high-purity adenostemmoic acid B from zanthoxylum acanthopodium

A high-purity, prickly prickly ash technology, applied in the direction of organic chemistry, can solve the problems of prickly prickly ash chemical composition research, no high-purity pecarpone, etc., and achieve the effect of reducing the number of extractions, simplifying the process, and increasing the extraction rate

Inactive Publication Date: 2012-03-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies on the chemical constituents of Zanthoxylum bungeanum, and there is no report on the process of extracting and preparing high-purity pistachioside from Zanthoxylum bungeanum in the existing literature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Prickly prickly pear rhizome, get 5kg and add 30L of 80% ethanol solution (containing 0.5% Tween 20), heat and reflux for extraction 2 times, each 4 hours, filter, merge the two extracts, concentrate under reduced pressure until no alcohol smell, the concentrated solution The pretreated D101 macroporous adsorption resin column was first eluted with deionized water until the eluent was colorless, and then eluted with 20% ethanol and 55% ethanol in turn. The 55% ethanol eluent was collected and concentrated under reduced pressure. Obtain the prickly ash extract. The prickly ash extract was purified by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-methanol-water (12:18:8:15) as the solvent system, the lower phase was the mobile phase, the upper phase was the stationary phase, and the collected Fractionation of pomegranate, recovery of solvent to obtain pomegranate, the purity of which was determined by HPLC method was 95.4%.

Embodiment 2

[0017] Prickly prickly pear rhizomes, get 5kg and add 50L of 65% ethanol solution (containing 1% Tween 80), heat and reflux for extraction 2 times, each 3 hours, merge the two extracts, concentrate under reduced pressure to no alcohol smell, and pass the concentrated solution through the pre-treatment method. The treated AB-8 macroporous adsorption resin column was first eluted with deionized water until the eluent was colorless, and then eluted with 10% ethanol and 80% ethanol in turn. The 80% ethanol eluent was collected and concentrated under reduced pressure. Obtain the prickly ash extract. The prickly ash extract was purified by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-methanol-water (15:20:15:7) as the solvent system, the lower phase was the mobile phase, the upper phase was the stationary phase, and the collected The fraction of pomegranate was fractionated, and the solvent was recovered to obtain pomegranate. The purity was 94.6% as determ...

Embodiment 3

[0019] Prickly prickly pear rhizomes, get 10kg and add 80L of 72% ethanol solution (containing 2% Tween 80), heat and reflux for extraction 2 times, extract 3 hours each time, collect the extract, concentrate under reduced pressure to no alcohol smell, and pass the concentrated solution through pretreatment. A good HPD100 macroporous adsorption resin column was first eluted with deionized water until the eluent was colorless, then eluted with 15% ethanol and 75% ethanol in turn, and the 75% ethanol eluent was collected and concentrated under reduced pressure to obtain Zanthoxylum bungeanum Extract. The prickly ash extract was purified by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-methanol-water (14:23:12:10) as the solvent system, the lower phase was the mobile phase, the upper phase was the stationary phase, and the collected Fractionation of pomegranate, recovery of solvent to obtain pomegranate, the purity of which was determined by HPLC method w...

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Abstract

The invention relates to a method for extracting high-purity adenostemmoic acid B from zanthoxylum acanthopodium. The method comprises the following three steps of: 1) ethanol extraction: crushing zanthoxylum acanthopodium rhizomes, adding 0.5 to 5 percent surfactant, performing reflux extraction by adopting ethanol, and concentrating the extract till ethanol smell does not exist; 2) macroporous resin adsorption: separating the obtained concentrate through macroporous adsorption resin, performing gradient elution by using water or ethanol, reclaiming ethanol from the eluent under reduced pressure, and obtaining an extract; and 3) high-speed countercurrent chromatography purification: further purifying the obtained extract by using high-speed countercurrent chromatography, and thus obtaining the adenostemmoic acid B with the purity of over 95 percent. Compared with the conventional extraction process, the method has the advantages that: after the surfactant is added, the extraction rate can be improved, the extraction frequency is reduced, a clear solution can be obtained, and an adsorption column is not blocked during filling; and the method has the advantages of simplicity, convenience, fastness, high preparation quantity, high product purity and the like, and is easy in popularization and use.

Description

technical field [0001] The invention belongs to the field of natural medicines, and in particular relates to a method for extracting high-purity pectin from Zanthoxylum bungeanum. Background technique [0002] Adenostemmoic acid B, molecular formula C 25 H 28 O 6 , with a molecular weight of 424.49, is a lignan compound, a white granular crystal, mp.102 ℃ (methanol). Pharmacological studies have shown that pomegranate has a central nervous system inhibitory effect. [0003] Prickly prickly ash, alias: wild prickly ash, rock pepper, derived from Rutaceae prickly prickly ash ( Zanthoxylum acanthopodium DC.), the root and fruit are used as medicine. Mainly distributed in Yunnan, it is spicy, numb and warm in nature. Functions and Indications: Warming the middle and dispelling cold, relieving pain, killing insects, contraception; Indicating stomach pain, rheumatism and joint pain, contraception, abdominal pain due to insect accumulation. However, there are few researches ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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