Preparation method of Nudaphantin A

A technology of pumiladin and pumiladin, which is applied in the field of preparation of pubisin A, can solve the problems of less research on tannin and less pulicin A, and achieve large preparation volume, small sample loss, The effect of reducing the throughput

Inactive Publication Date: 2013-08-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wu Xia et al. found that the methanol extract from the rhizome of Pineapple japonica has insecticidal activity against Drosophila larvae of Acetobacter, but there are few studies on tannins, so it is necessary to develop a method for preparing tannins from Pineapple japonica , which is of great significance to the expansion of drug sources and the comprehensive utilization of Pinnaea plants
[0004] At present, there are few studies on pinchalin A, and there is no relevant report on the extraction process of pinchryl A in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Pulverize the rhizome of Pinnaea japonica, get 1kg, carry out ultrasonic extraction with 12kg75% ethanol solution, the ultrasonic frequency is 50KHz, extract 3 times, each time 0.5h, the extract is concentrated to obtain the ethanol crude extract of Pincus japonicus rhizome, use Ethyl acetate extracts the crude extract, filters, and concentrates the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent is evaporated and put on a silica gel column. The dichloromethane-methanol ratio is 15:1, 7: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 5:3:8 : 4 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, and the main engine rotating speed is 800rpm, and the flow rate of the mo...

Embodiment 2

[0022] Pulverize the rhizome of P. japonicum, take 1kg, carry out ultrasonic extraction with 10kg70% ethanol solution, the ultrasonic frequency is 45KHz, extract 2 times, each time 1.5h, the extract is concentrated, and obtain the ethanol crude extract of P. japonica rhizome, use The crude extract was extracted with ethyl acetate, filtered, and the filtrate was concentrated under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent was evaporated and put on a silica gel column. The dichloromethane-methanol ratio by volume was 17:1, 9: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 3:2:6 : 4 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, the main engine rotating speed is 750rpm, and the fl...

Embodiment 3

[0024] Pulverize the rhizome of Pinnaea japonica, take 1kg, and carry out ultrasonic extraction with 8kg60% ethanol solution, the ultrasonic frequency is 70KHz, extract 2 times, each time for 1.5h, and concentrate the extract to obtain the crude ethanol extract of the rhizome of Pineapple japonica, use Ethyl acetate extracts the crude extract, filters, and concentrates the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent is evaporated and put on a silica gel column. The dichloromethane-methanol ratio by volume is 16:1, 8: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 3:2:6 : 2 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, and the rotating speed of the main engine is 7...

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Abstract

The invention belongs to the technical field of extraction of effective ingredients of plants and relates to a preparation method of Nudaphantin A. The preparation method comprises the following steps of: crushing Nuphar japonica rootstock; performing ultrasonic extraction by using an ethanol solution to obtain an alcohol extract; extracting the alcohol extract by using ethyl acetate; filtering; concentrating the filtrate under reduced pressure; mixing with a small amount of silica gel; volatilizing the solvent; passing through a silica gel column; performing dichloromethane-methanol gradient elution; collecting the eluent; concentrating; separating and purifying by a high-speed counter-current chromatography method; and carrying out freeze drying to obtain the product. The preparation method is simple to operate and low in energy consumption and the product has high purity.

Description

technical field [0001] The invention belongs to the technical field of extraction of effective plant components, and relates to a preparation method of pincitin A. Background technique [0002] Nudaphantin A (Nudaphantin), the molecular formula is C 41 h 30 o 26 , with a molecular weight of 938.67, is from the Nymphaeaceae plant Japanese pinnaea Nuphar japonicum DC. The tannin substances isolated from the rhizomes, the melting point of impenin A is 243-245°C, and it is a white powder; pharmacological studies have shown that impenin A has antibacterial effects on Staphylococcus aureus and Sarcchomyces cerevisiae , showed inhibitory activity against topoisomerase type Ⅱ, IC 50 0.2 μM. [0003] Japanese duckweed is a perennial rhizome herbaceous plant widely distributed in the temperate zone of the northern hemisphere. It has been used as medicine in Asia and contains a variety of alkaloids and tannins. Wu Xia et al. found that the methanol extract from the rhizomes of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/08
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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