A stachydrine preparing method

A stachydine and preparation-type technology, which is applied in the field of separation and preparation of stachydine, can solve the problems of rare stachydine purification methods, patents or literature reports on the industrialization of stachydine, and the like, and achieves short preparation period, easy Operation, solving the effect of low efficiency

Inactive Publication Date: 2016-10-26
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the purification method of stachydrine is rare, and there is no patent or literature report suitable for the industrialized method of producing stachydrine in large quantities.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The pulverized motherwort powder was placed in a supercritical fluid extraction device, with ethanol accounting for 4% of the total extractant volume as the entrainer, and CO 2 , at extraction pressure 20MPa, extraction temperature 40°C, CO 2 Extraction is performed under the condition of 20L / h flow rate, and the extract is collected; the extract is concentrated through an ultrafiltration membrane with a molecular weight cut-off of 2000 and a nanofiltration membrane with a molecular weight cut-off of 300, and the operating pressure is 0.7MPa, vacuum-dried, Obtain the crude extract; adopt preparative liquid chromatography to separate and purify the stachydrine in the crude extract, use 75% methanol solution as the mobile phase, and use ultraviolet on-line monitoring to collect the stachydrine component; the stachydrine component is subjected to vacuum Concentrate and crystallize methanol to obtain stachydrine with a purity of 96.3%.

Embodiment 2

[0021] The pulverized motherwort powder was placed in a supercritical fluid extraction device, with ethanol accounting for 4% of the total extractant volume as the entrainer, and CO 2 , at extraction pressure 25MPa, extraction temperature 45°C, CO 2 Extraction is carried out under the condition of 25L / h flow rate, and the extract is collected; the extract is concentrated by ultrafiltration with a molecular weight cut-off of 3000 ultrafiltration membrane and a nanofiltration membrane with a molecular weight cut-off of 300, and the operating pressure is 1.0MPa, vacuum-dried, Obtain the crude extract; adopt preparative liquid chromatography to separate and purify the stachydrine in the crude extract, use 80% methanol solution as the mobile phase, and monitor the ultraviolet on-line to collect the stachydrine component; the stachydrine component is subjected to vacuum Concentrate and crystallize methanol to obtain stachydrine with a purity of 98.1%.

Embodiment 3

[0023] The pulverized motherwort powder was placed in a supercritical fluid extraction device, with ethanol accounting for 4% of the total extractant volume as the entrainer, and CO 2 , at extraction pressure 30MPa, extraction temperature 50°C, CO 2 Extraction is carried out under the condition of 30L / h flow rate, and the extract is collected; the extract is concentrated through an ultrafiltration membrane with a molecular weight cut-off of 2500 and a nanofiltration membrane with a molecular weight cut-off of 300, and the operating pressure is 1.5MPa, vacuum-dried, Obtain the crude extract; adopt preparative liquid chromatography to separate and purify the stachydrine in the crude extract, use 82% methanol solution as the mobile phase, and monitor the ultraviolet on-line to collect the stachydrine component; the stachydrine component is subjected to vacuum Concentrate and crystallize methanol to obtain stachydrine with a purity of 97.2%.

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PUM

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Abstract

The invention relates to a stachydrine preparing method simple in operation and low in pollution. The method includes (1) adding crushed motherwort herb powder into a supercritical fluid extraction device, and performing supercritical fluid extraction to obtain an extract liquid, (2) allowing the extract liquid to pass through a membrane separation system, concentrating and drying to obtain a crude extract product, (3) separating and purifying stachydrine in the crude extract product through preparative liquid chromatography, monitoring on line with ultraviolet, and collecting the stachydrine component, and (4) subjecting the stachydrine component to vacuum concentration, and crystallizing with methanol to obtain the stachydrine. The stachydrine prepared by the method is high in product purity and prone to industrial scale-up.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and relates to a method for separating and preparing stachydrine from motherwort. Background technique [0002] Stachydrine, also known as proline betaine, is the simplest pyrrole alkaloid, white needle crystal, soluble in water, methanol, ethanol, dilute acid, hot chloroform, almost insoluble in ether, acetone, cold chloroform and petroleum ether. Stachydrine is one of the main active ingredients of the medicinal plant Motherwort. It has good medicinal value and has the functions of stimulating the uterus, improving blood rheology, and antithrombotic effects. [0003] Motherwort is the fresh or dry aboveground part of the Lamiaceae Leonurus plant, formerly known as Chiwei, aliased as Motherwort, Bitter Grass, Kuncao, etc. It tastes pungent, slightly bitter, and slightly cold in nature. The effect of regulating blood stasis, inducing diuresis a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/16
CPCC07D207/16Y02P20/54
Inventor 杨成东
Owner NANJING ZELANG MEDICAL TECH
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