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Phyllanthostatin A preparation process

A preparation process and drying technology, which is applied in the field of preparation process of Phyllophyllum Stetin A, to achieve high separation efficiency and improve product purity

Inactive Publication Date: 2013-08-07
NANJING ZELANG MEDICAL TECH
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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 phyllastine A, so providing a preparation process of phyllastine A is of great significance for the development of medicinal material resources and pharmacological research containing phyllastine A

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 38°C, the pressure is 25MPa, and CO 2 The flow rate is 18L / h. After the environment in the extraction tank is stable, 1500ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 2 hours of extraction, analysis is carried out at a temperature of 35°C and a pressure of 8.5MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether 4 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use 5 times the amount of the extract to pack silica gel (column diameter to height ratio 1:10), put the mixed sample silica gel on the top of the co...

Embodiment 2

[0014] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 45°C, the pressure is 28MPa, and CO 2 The flow rate is 20L / h. After the environment in the extraction tank is stabilized, 750ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 3 hours of extraction, analysis is performed. The analysis temperature is 35°C and the pressure is 8.5MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether for 5 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use 4 times the amount of silica gel to pack the extract into a column (column diameter to height ratio 1:8), put the mixed sample si...

Embodiment 3

[0016] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 55°C, the pressure is 29MPa, and CO 2 The flow rate is 26L / h. After the environment in the extraction tank is stabilized, 1000ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 2.5 hours of extraction, analysis is performed. The analysis temperature is 40°C and the pressure is 9MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether 4 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use silica gel 6 times the amount of the extract to pack the column (column diameter to height ratio 1:15), put the mixed sample silica ...

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PUM

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Abstract

The invention discloses a Phyllanthostatin A preparation process which comprises the following steps: pulverizing dried roots of Phyllanthus acuminatus Vahl. to 40 meshes, putting into an extraction kettle, introducing liquid CO2 and entrainer, and performing supercritical extraction to obtain an extract; performing ether extraction on the extract multiple times, and concentrating the obtained extract liquid to obtain ether extractum; and performing silica gel column chromatography on the ether extractum, performing n-hexane-ethyl acetate gradient elution, performing rotary evaporation and concentration on the eluate, and drying to obtain a Phyllanthostatin A product. The method has the advantages of high efficiency and low pollution, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction of effective components of traditional Chinese medicines, and relates to a preparation process of Phyllostatin A. Background technique [0002] Phyllantostatin A is a lignan compound with the molecular formula C 29 h 30 o 13 , with a molecular weight of 586.55, an amorphous solid, mp.127-130°C. Stetin A is mainly derived from Phyllanthus acuminate Phyllanthus acuminatus Root of Vahl. Pharmacological studies have shown that phyllostatin has cytostatic activity and inhibits the growth of PS leukemia cells in vitro, ED 50 4 μg / mL. [0003] At present, there are few studies on phyllastine A, so providing a preparation process of phyllastine A is of great significance for the development of medicinal material resources and pharmacological research containing phyllastine A. Contents of the invention [0004] The purpose of the present invention is to provide a preparation process of Phyllost...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/08
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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