A method for purifying withaferin a

A technology of withaferin and macroporous resin, which is applied in the field of natural medicinal chemistry, can solve the problems of silica gel column separation sample loss, easy emulsification of extraction solvent, and difficult quantitative production, etc., to overcome dead adsorption of samples, large amount of preparation, and simple operation Effect

Inactive Publication Date: 2011-11-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many technical defects in these existing methods, such as the extraction solvent is easy to emulsify, the extraction effect is poor, and the silica gel column separation sample loss is serious, the yield and yield are low, and it is difficult to quantitatively produce

Method used

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  • A method for purifying withaferin a

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Embodiment 1

[0014] The raw material of Indian ginseng is crushed, 2kg is added to the ultrasonic extraction tank, 10 times the amount of 90% methanol is added for ultrasonic extraction, the power is 2kw, the frequency is 40kHz, the extraction is 30min, the liquid is filtered, and 6 times the amount of methanol is added for 30min, and the two extractions are combined The liquid is decompressed to recover methanol, add appropriate amount of water to disperse, add 300g HZ816 macroporous resin for adsorption, first take 1.2L of 60% methanol solution to elute impurities, and then use 1.5L of 90% methanol solution to elute, collect the eluate and concentrate to obtain paste. Mix chloroform, methanol, and water in a ratio of 5:5:3, let stand to separate layers, take the upper phase and inject it into a high-speed countercurrent chromatographic column, turn on the high-speed countercurrent chromatograph, adjust the rotation speed to 900rpm, and pump it into the lower phase at a flow rate of 6ml / mi...

Embodiment 2

[0016] Indian ginseng raw material is crushed, take 2kg and put it into the ultrasonic extraction tank, add 8 times the amount of 80% methanol for ultrasonic extraction, turn on the power 2kw, frequency 640kHz, extract for 30min, extract twice, combine the extracts to recover methanol under reduced pressure, add appropriate amount of water, add Adsorb in 300gHZ816 macroporous resin, first take 1.5L of 40% methanol solution to elute impurities, and then use 1.52L of 99% methanol solution to elute, collect and concentrate the eluate to obtain extract. Take chloroform, methanol, and water and mix them in a ratio of 4:3:2, let them stand for stratification, take the upper phase and inject it into a high-speed countercurrent chromatography column, turn on the high-speed countercurrent chromatography, adjust the rotation speed to 700rpm, and pump it into the lower phase at a flow rate of 8ml / min at the same time. After the whole system is dynamically balanced, the flow rate of the mo...

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Abstract

The invention belongs to the field of natural medicinal chemistry and discloses a method for purifying withaferin A. The method is: take the Indian ginseng raw material and grind it, add 6-10 times the amount of 80-90% methanol for ultrasonic extraction 2-3 times, extract the solution under reduced pressure to recover the reagent, add the concentrated solution to the macroporous resin for adsorption, first use 4-5 times the volume 40-60% methanol solution to elute impurities, and then use 3-5 times the amount of 90-99% methanol solution to elute. The eluent recovers methanol to obtain extract, and then separates by high-speed countercurrent chromatography, collects the target components according to the map, and concentrates Refrigerate and crystallize to a small volume, and dry to obtain high-purity withaferin A. Purifying withaferin A by adopting the present invention has simple and easy-to-operate process, short cycle, product purity above 98%, and is suitable for industrialized preparation.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method for purifying withaferin A. Background technique [0002] Withaferin A (Withaferin A) is a lactone compound, CAS number: 5119-48-2, melting point 252-253°C, molecular formula C 28 h 38 o 6 , molecular weight 470.6, molecular structure formula is: [0003] [0004] Studies have shown that withaferin A is similar to steroid hormones in the human body, and has dual regulatory effects, that is, when the hormone is excessive in the body, it occupies the cell membrane receptor site and inhibits it, and when the hormone level is low, it can be transformed into Corresponding hormones, whose good adaptogenicity can help the body generate non-specific immunity in various stresses, recovery and environmental changes. It also has significant antibacterial, fungal, tumor and inflammation effects. [0005] The existing methods for purifying withaferin A mostly use In...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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