Method for preparing pallidisetin A

A technology for moss blondii and cyanidin, which is applied in the field of preparing cyanidin A, and achieves the effects of high yield, simple operation and large preparation amount

Inactive Publication Date: 2013-08-28
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are few studies on chrysalis chrysogenin A, so providing a preparation method of chrysalis chrysogenin A is of great significance for the development and pharmacological research of chrysanthemum chrysogenin A-containing medicinal material resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Get moss goldensells medicinal material and pulverize, control particle diameter to be 60 orders, take by weighing 500g, be 1:10 to add 85% ethanol solution with solid-liquid volume ratio, adopt ultra-high pressure method to extract, extraction pressure is 400MPa, and holding time is 3.5min, repeat 3 times, combine extracts, concentrate under reduced pressure to obtain extract extract, extract 3 times with n-butanol, combine n-butanol extract, concentrate to obtain extract extract, mix extract with a small amount of neutral magnesium oxide Mix the sample, dry it at low temperature, load the sample to a 100-mesh neutral magnesium oxide low-pressure column (column pressure is 6 bar, column diameter-to-height ratio is 1:7), and use petroleum ether-acetone at a volume ratio of 20:1-3:1. Gradient elution, collect each part of the eluate, concentrate and dry the petroleum ether-acetone (3:1) eluate to obtain the crude product. The crude product was separated and purified by p...

Embodiment 2

[0018] Get moss goldensells medicinal material and pulverize, control particle diameter to be 60 orders, take by weighing 500g, be 1:18 to add 85% ethanol solution with solid-liquid volume ratio, adopt ultra-high pressure method to extract, extraction pressure is 400MPa, and holding time is 5min, repeated 3 times, combined extracts, concentrated under reduced pressure to obtain extract extract, extracted 4 times with n-butanol, combined n-butanol extract, concentrated to obtain extract extract, mixed extract with a small amount of neutral magnesium oxide Samples were dried at low temperature, loaded onto a 200-mesh neutral magnesium oxide low-pressure column (column pressure 5 bar, column diameter-to-height ratio 1:12), and a gradient was carried out with petroleum ether-acetone at a volume ratio of 20:1-3:1 For elution, collect each part of the eluate, concentrate and dry the petroleum ether-acetone (3:1) eluate to obtain a crude product. The crude product was separated and p...

Embodiment 3

[0020] Get moss goldensells medicinal material and pulverize, control particle diameter to be 60 orders, take by weighing 500g, be 1:15 to add 95% ethanol solution with solid-liquid volume ratio, adopt ultra-high pressure method to extract, extraction pressure is 400MPa, and holding time is 3 min, repeat 3 times, combine extracts, concentrate under reduced pressure to obtain extract extract, extract 3 times with n-butanol, combine n-butanol extract, concentrate to obtain extract extract, mix extract with a small amount of neutral magnesium oxide Mix the sample, dry at low temperature, load the sample to a 200-mesh neutral magnesium oxide low-pressure column (column pressure is 7.5bar, column diameter-to-height ratio is 1:10), and use petroleum ether-acetone at a volume ratio of 20:1-3:1 Carry out gradient elution, collect each part of the eluate, concentrate and dry the petroleum ether-acetone (3:1) eluate to obtain the crude product. The crude product was separated and purifi...

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Abstract

The invention discloses a method for preparing pallidisetin A. The method comprises the following steps of: crushing polytrichum pallidisetum funoh, extracting by using an ethanol solution under ultrahigh pressure, combining the extracts, concentrating and extracting by using n-butyl alcohol, feeding the extracting solution into a magnesium oxide column, carrying out gradient eluting by using a petroleum ether-acetone mixture solution, concentrating the eluent, and subsequently further purifying the eluent by using high performance liquid chromatography so as to obtain the pallidisetin A. The method is simple to operate, large in preparation quantity, high in yield, high in product purity and applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine chemistry, and relates to a method for preparing chrysanthemum A. Background technique [0002] Pallidisetin A, the molecular formula is C 23 h 18 o 3 , with a molecular weight of 342.39, colorless flaky crystals, mp.233°C. Mainly found in the family Polytrichaceae (Polytrichaceae) Golden hair moss Polytrichum pallidisetum Funoh. Pharmacological studies have shown that trichosanthin A has cytotoxic activity. The ED50 of human melanoma cancer cell RPMI-7951 and malignant glioma U-251MG is 1.0 μg / mL. [0003] At present, there are few studies on chrysogenin A, so providing a preparation method of chrysalis is of great significance for the development of blondin A-containing medicinal material resource development and pharmacological research of chrysanthemum. Contents of the invention [0004] The purpose of the present invention is to provide a method for preparing chr...

Claims

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Application Information

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IPC IPC(8): C07D307/79
Inventor苏刘花万冬梅
OwnerNANJING ZELANG AGRI DEV