CN106045890A - A stachydrine preparing method - Google Patents
A stachydrine preparing method Download PDFInfo
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- CN106045890A CN106045890A CN201610306944.0A CN201610306944A CN106045890A CN 106045890 A CN106045890 A CN 106045890A CN 201610306944 A CN201610306944 A CN 201610306944A CN 106045890 A CN106045890 A CN 106045890A
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- Prior art keywords
- stachydrine
- extract
- crude extract
- component
- supercritical fluid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
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
The invention belongs to Chinese medicine extraction separation technology field, relate to a kind of from Herba Leonuri separation prepare the side of stachydrine
Method.
Background technology
Stachydrine, also known as proline glycine betaine, is simplest pyrrolidine alkaloid, for white, needle-shaped crystals, is dissolved in water, first
Alcohol, ethanol, diluted acid, hot chloroform, be practically insoluble in ether, acetone, cold chloroform and petroleum ether.Stachydrine is medicinal plants Herba Leonuri
One of main active, have good medical value, there is excited uterus, improve hemorheology, antithrombotic effect.
Herba Leonuri is the fresh or dry aerial parts of Labiatae mother wort plant, original name motherwort, another name Herba Leonuri Chinese mugwort, hardship
Grass, Herba Leonuri etc., its acrid in the mouth, micro-hardship, cold nature, enter pericardium, Liver Channel, there is invigorate blood circulation the tune stasis of blood, effect of inducing diuresis to remove edema.Clinically
Treatment for diseases such as menoxenia, stasis of blood pain in puerperal, cardiovascular and cerebrovascular disease, hematopathys.
At present, the purification process of stachydrine is rarely found, not yet finds to be suitable for preparing in a large number the industrial method of stachydrine
Patent or document report.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of stachydrine.
The present invention is achieved by the following technical programs:
(1) will pulverize after Herba Leonuri powder be placed in supercritical fluid extraction equipment, with account for total extractant volume 4% second
Alcohol is entrainer, is passed through CO2, at extracting pressure 20～30MPa, extraction temperature 40～50 DEG C, CO2Flow velocity be 20～30L/h
Under the conditions of extract, collect extract；
(2) it is the nanofiltration of 300 by extract by ultrafilter membrane ultrafiltration and the molecular cut off that molecular cut off is 2000～3000
Membrance concentration, operation pressure is 0.7～1.5MPa, and vacuum drying obtains crude extract；
(3) using the stachydrine in the isolated and purified crude extract of preparative liquid chromatography, on-line ultraviolet is monitored, and collects stachydrine group
Point；
(4) stachydrine component is concentrated in vacuo, methanol crystallization, obtains stachydrine.
In described step (3) preparative liquid chromatography with 75～82% methanol solution for flowing phase.
This method good effect is:
(1) this method uses supercritical fluid extraction, mild condition, it is to avoid traditional method localized hyperthermia is to Product Activity
Adverse effect；
(2) this method uses membrane separation technique, can effectively remove plurality of impurities, and will not destroy the biological activity of effective ingredient；
(3) this method uses preparative liquid chromatography, and yield is high, preparation amount is big, manufacturing cycle is short, solves column chromatography efficiency low
And with serious pollution technological deficiency；
(4) operation of this method processing step is relatively simple, easily operates, and products obtained therefrom purity is high.
Further illustrate the present invention below in conjunction with detailed description of the invention, but the scope of protection of present invention is not limited to
In following embodiments.
Detailed description of the invention
Embodiment 1:
Will pulverize after Herba Leonuri powder be placed in supercritical fluid extraction equipment, with account for total extractant volume 4% ethanol be
Entrainer, is passed through CO2, at extracting pressure 20MPa, extraction temperature 40 DEG C, CO2Flow velocity be to extract under conditions of 20L/h,
Collect extract；It is the NF membrane of 300 by extract by ultrafilter membrane ultrafiltration and the molecular cut off that molecular cut off is 2000
Concentrating, operation pressure is 0.7MPa, vacuum drying, obtains crude extract；Use in the isolated and purified crude extract of preparative liquid chromatography
Stachydrine, monitors for flowing phase, on-line ultraviolet with 75% methanol solution, collects stachydrine component；Stachydrine component is carried out vacuum
Concentrating, methanol crystallization, obtain stachydrine, its purity is 96.3%.
Embodiment 2:
Will pulverize after Herba Leonuri powder be placed in supercritical fluid extraction equipment, with account for total extractant volume 4% ethanol be
Entrainer, is passed through CO2, at extracting pressure 25MPa, extraction temperature 45 DEG C, CO2Flow velocity be to extract under conditions of 25L/h,
Collect extract；It is the NF membrane of 300 by extract by ultrafilter membrane ultrafiltration and the molecular cut off that molecular cut off is 3000
Concentrating, operation pressure is 1.0MPa, vacuum drying, obtains crude extract；Use in the isolated and purified crude extract of preparative liquid chromatography
Stachydrine, monitors for flowing phase, on-line ultraviolet with 80% methanol solution, collects stachydrine component；Stachydrine component is carried out vacuum
Concentrating, methanol crystallization, obtain stachydrine, its purity is 98.1%.
Embodiment 3:
Will pulverize after Herba Leonuri powder be placed in supercritical fluid extraction equipment, with account for total extractant volume 4% ethanol be
Entrainer, is passed through CO2, at extracting pressure 30MPa, extraction temperature 50 DEG C, CO2Flow velocity be to extract under conditions of 30L/h,
Collect extract；It is the NF membrane of 300 by extract by ultrafilter membrane ultrafiltration and the molecular cut off that molecular cut off is 2500
Concentrating, operation pressure is 1.5MPa, vacuum drying, obtains crude extract；Use in the isolated and purified crude extract of preparative liquid chromatography
Stachydrine, monitors for flowing phase, on-line ultraviolet with 82% methanol solution, collects stachydrine component；Stachydrine component is carried out vacuum
Concentrating, methanol crystallization, obtain stachydrine, its purity is 97.2%.
Claims (2)
1. the preparation method of a stachydrine, it is characterised in that comprise the following steps:
(1) will pulverize after Herba Leonuri powder be placed in supercritical fluid extraction equipment, with account for total extractant volume 4% second
Alcohol is entrainer, is passed through CO2, at extracting pressure 20～30MPa, extraction temperature 40～50 DEG C, CO2Flow velocity be 20～30L/h
Under the conditions of extract, collect extract；
(2) it is the nanofiltration of 300 by extract by ultrafilter membrane ultrafiltration and the molecular cut off that molecular cut off is 2000～3000
Membrance concentration, operation pressure is 0.7～1.5MPa, and vacuum drying obtains crude extract；
(3) using the stachydrine in the isolated and purified crude extract of preparative liquid chromatography, on-line ultraviolet is monitored, and collects stachydrine group
Point；
(4) stachydrine component is concentrated in vacuo, methanol crystallization, obtains stachydrine.
The preparation method of a kind of stachydrine the most according to claim 1, it is characterised in that preparative in described step (3)
Liquid chromatograph with 75～82% methanol solution for flowing phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610306944.0A CN106045890A (en) | 2016-05-11 | 2016-05-11 | A stachydrine preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610306944.0A CN106045890A (en) | 2016-05-11 | 2016-05-11 | A stachydrine preparing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106045890A true CN106045890A (en) | 2016-10-26 |
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ID=57176347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610306944.0A Pending CN106045890A (en) | 2016-05-11 | 2016-05-11 | A stachydrine preparing method |
Country Status (1)
| Country | Link |
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| CN (1) | CN106045890A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928115A (en) * | 2017-03-29 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract stachydrine hydrochloride in motherwort |
| CN108586308A (en) * | 2018-06-15 | 2018-09-28 | 南京中医药大学 | A kind of method that film combination refines both sexes alkaloid |
-
2016
- 2016-05-11 CN CN201610306944.0A patent/CN106045890A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928115A (en) * | 2017-03-29 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract stachydrine hydrochloride in motherwort |
| CN108586308A (en) * | 2018-06-15 | 2018-09-28 | 南京中医药大学 | A kind of method that film combination refines both sexes alkaloid |
| CN108586308B (en) * | 2018-06-15 | 2021-06-22 | 南京中医药大学 | Method for refining amphoteric alkaloid by membrane combination |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161026 |
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| WD01 | Invention patent application deemed withdrawn after publication |