CN105017355B - The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of 6 ' O - Google Patents
The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of 6 ' O Download PDFInfo
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- CN105017355B CN105017355B CN201510427890.9A CN201510427890A CN105017355B CN 105017355 B CN105017355 B CN 105017355B CN 201510427890 A CN201510427890 A CN 201510427890A CN 105017355 B CN105017355 B CN 105017355B
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Abstract
Specification digest：The present invention relates to study of tcm new drug field, in particular to the positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of 6 ' O of one kind.Raw materials used is the Chinese medical extract that the trans cinnamyl catalpol contents of 6 ' O are more than 35%（It can be patent：201110400683.6 " methods prepared by 10 fragrant pod acyl Catalpols " introduced prepare extract remaining after 10 fragrant pod acyl Catalpols, can also be ethanol, methanol eddy extraction, the plant extracts for containing the trans cinnamyl Catalpols of 6 ' O obtained through the mode such as petroleum ether or ethyl acetate extraction）, its purity is made by the method for positive pressurized column chromatography>95%.Twice laid of the present invention, energy-conserving and environment-protective, filler is cheap, and cost is low, and single treatment sample size is big, and efficiency high is with short production cycle, the features such as solvent recovery is fast, is adapted to industrial-scale production.
Description
Technical field
The present invention relates to study of tcm new drug field, in particular to the positive of the trans cinnamyl Catalpols of 6 '-O- of one kind
Pressurized column chromatography preparation method.
Background technology
The trans cinnamyl Catalpols of 6 '-O- are the main components in traditional Chinese medicine Radix picrorrhizae.The trans cinnamyl Catalpol tools of 6 '-O-
There are the multiple efficacies such as antibacterial, liver protection, cholagogic, hypoglycemic.The external mixture by the trans cinnamyl Catalpols of 6 '-O- and other materials
Applied to clinic, the country develops the total glycosides of picrorhiza iridoid in recent years（With the trans cinnamyl Catalpols of 6 '-O- and the fragrant first of 10-
Acyl Catalpol is main pharmacodynamics composition）, comparatively speaking, the simple trans cinnamyl Catalpols of 6 '-O- are applied to clinical drug effect will more
Plus clearly, side effect is smaller, and drug safety will be more secure with validity.Through retrieval, it is trans that domestic patent is related to 6 '-O-
Prepared by cinnamyl Catalpol has：2007101643215：Using normal pressure column chromatography, technique is simple, but influence efficiency；
2013106189968：Using reverse phase filler chromatographic technique, efficiency high but costly, presently disclosed technique use pressurization
Normal-phase chromatography separation method, big with single treatment sample size compared to above-mentioned two patent, filler is cheap, and efficiency high uses work
The advantages of skill equipment is advanced.
The content of the invention
The raw materials used present invention is Chinese medical extract of the trans cinnamyl catalpol contents of 6 '-O- more than 35%（It can be patent
（The patent No.：201110400683.6）" method prepared by 10- perfume pod acyl Catalpols " introduced is prepared after the fragrant pod acyl Catalpols of 10-
Remaining extract or other contain the plant extracts of the trans cinnamyl Catalpols of 6 '-O-）, pass through positive pressured column
The method of chromatography makes its purity>95%.
Take patent（The patent No.：201110400683.6）It is prepared by " method prepared by 10- perfume pod acyl Catalpols " introduced
Remaining extract after 10- perfume pod acyl Catalpols, the content of the trans cinnamyl Catalpols of 6 '-O- is between 40% ~ 50% after testing（Or its
He contains the plant extracts that the trans cinnamyl Catalpol amounts of 6 '-O- are more than 35%）, ethanol dissolving, which adds, mixes sample silica gel mixed sample, loads sample
Capo.
Take chromatographic silica gel to load chromatographic column, 3-5 bed volume of chromatographic column is rinsed with mobile phase, by sample column and chromatographic column
Be together in series, rinsed with mobile phase, mobile phase be hexamethylene, chloroform, ethyl acetate, ethanol, the one or two kinds of solvents of methanol with
Certain proportion is used in mixed way.50 ~ 150ml/min of flow velocity.
Set wavelength as 265nm or 235nm or 282nm using dual wavelength ultraviolet detector, detected, to detect peak response
It is worth for according to eluent is collected, eluent is drying to obtain.
Specific embodiment
Specific examples below can substantially obtain purity>The 95% trans cinnamyl Catalpols of 6 '-O-, but according to professional skill
Art knowledge can be finely adjusted to obtain same effect, all changes without prejudice to spirit of the present invention to presently disclosed mobile phase
All it is considered as present invention.
Embodiment 1
Take patent（The patent No.：201110400683.6）It is prepared by " method prepared by 10- perfume pod acyl Catalpols " introduced
Remaining extract 25g after 10- perfume pod acyl Catalpols, the content of the trans cinnamyl Catalpols of 6 '-O- is 47% after testing, molten with ethanol
Add 37.5g to mix sample silica gel mixed sample after solution, load sample column.
Take 120g chromatographic silica gels to load chromatographic column, use mobile phase（Chloroform：Methanol=20:1）Rinse 3-5 post bed of chromatographic column
Volume, sample column is got up with chromatography column in series, is rinsed with mobile phase, and flow velocity 50ml/min, pressure is 78psi.
With dual wavelength ultraviolet detector（It is 265nm to set its wavelength 1, and wavelength 2 is 235nm）Detected, to detect peak
Response is, according to collection eluent, recycling design, to obtain the trans g of cinnamyl Catalpol 10.3 of 6 '-O-, high performance liquid chromatography inspection
It is 94.6% to survey its purity.
Embodiment 2
Take patent（The patent No.：201110400683.6）" method prepared by 10- perfume pod acyl Catalpols " introduced prepares 10-
Remaining extract 40g after fragrant pod acyl Catalpol, the content of the trans cinnamyl Catalpols of 6 '-O- is 36% after testing, and ethanol dissolving adds
60g mixes sample silica gel mixed sample, loads sample column.
Take 180g chromatographic silica gels to load chromatographic column, use mobile phase（Chloroform：Ethanol=18:1）Rinse 3-5 post bed of chromatographic column
Volume, sample column is got up with chromatography column in series, is rinsed with mobile phase, and flow velocity 80ml/min, pressure is 85psi.
Wavelength 1 is set to be 265nm with dual wavelength ultraviolet detector, wavelength 2 is 282nm, is detected, to detect peak response
It is worth for according to eluent is collected, recycling design obtains the trans cinnamyl Catalpol 11.0g of 6 '-O-, and high performance liquid chromatography detects that its is pure
Spend for 96.0%.
Embodiment 3
Take patent（The patent No.：201110400683.6）It is prepared by " method prepared by 10- perfume pod acyl Catalpols " introduced
Remaining extract 22g after 10- perfume pod acyl Catalpols, the content of the trans cinnamyl Catalpols of 6 '-O- is 42% after testing, molten with ethanol
Add 34g to mix sample silica gel mixed sample after solution, load sample column.
120g chromatographic silica gels are taken to load chromatographic column, with mobile phase ethyl acetate rinse 3-5 bed volume of chromatographic column, by sample
Capo gets up with chromatography column in series, is rinsed with mobile phase, and flow velocity 120ml/min, pressure is 90psi.
With dual wavelength ultraviolet detector（It is 235nm to set its wavelength 1, and wavelength 2 is 282nm）Detected, to detect peak
Response is, according to collection eluent, recycling design, to obtain the trans cinnamyl Catalpol 8.3g of 6 '-O-, high performance liquid chromatography detection
Its purity is 95.2%.
Claims (4)
1. the positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of-O- of one kind 6 ', it is characterised in that fragrant to prepare 10-
Remaining extract is raw material after pod acyl Catalpol, wherein the content of the trans cinnamyl Catalpols of 6 '-O- is between 40%-50%, ethanol
After dissolving, sample is uniformly mixed with 100-200 mesh silica gel, dries pulverizing crosses 60 mesh sieves, and dry method loads sample column, by sample column and chromatography
Post is connected, and is rinsed with mobile phase, is collected corresponding eluent, be drying to obtain.
2. one kind 6 as claimed in claim 1’The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of-O-, its feature exists
In raw material and silica gel weight ratio are 1 when mixing sample：5-2：1.
3. one kind 6 as claimed in claim 1’The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of-O-, its feature exists
In setting wavelength as any two wavelength in 235nm, 265nm, 282nm using dual wavelength ultraviolet detector when collecting eluent.
4. one kind 6 as claimed in claim 1’The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of-O-, its feature exists
In chromatographic silica gel used in chromatographic column is 200-400 mesh, and mobile phase is：Hexamethylene, chloroform, ethyl acetate, ethanol, methanol are a kind of
Or two kinds of solvents are used in mixed way with certain proportion, pressurized pump system pressure is 80-200 Psi, and flow velocity is 50-130ml/min.
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| CN201510427890.9A CN105017355B (en) | 2015-07-21 | 2015-07-21 | The positive pressurized column chromatography preparation method of the trans cinnamyl Catalpols of 6 ' O |
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| CN105017355B true CN105017355B (en) | 2017-10-24 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186627A (en) * | 2004-12-15 | 2008-05-28 | 周亚伟 | Method for preparing picroside I |
| CN102516332A (en) * | 2011-12-06 | 2012-06-27 | 济南玉托金医药科技有限公司 | Preparation method of 10-vanilloyl catalpol |
| CN103601769A (en) * | 2013-11-27 | 2014-02-26 | 扬子江药业集团有限公司 | Preparation process for extracting, separating and purifying picroside I and picroside II from Picrorrhiza Kurrooa Royleex Benth |
| CN104693253A (en) * | 2015-03-30 | 2015-06-10 | 济南东源生物医药技术有限公司 | Industrial preparation method for high-purity 6'-O-trans-cinnamyl catalpol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005077392A1 (en) * | 2004-01-19 | 2005-08-25 | Ranbaxy Laboratories Limited | Herbal formulation comprising extracts of withania, tinospora and picrorhiza as a pediatric tonic |
-
2015
- 2015-07-21 CN CN201510427890.9A patent/CN105017355B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186627A (en) * | 2004-12-15 | 2008-05-28 | 周亚伟 | Method for preparing picroside I |
| CN102516332A (en) * | 2011-12-06 | 2012-06-27 | 济南玉托金医药科技有限公司 | Preparation method of 10-vanilloyl catalpol |
| CN103601769A (en) * | 2013-11-27 | 2014-02-26 | 扬子江药业集团有限公司 | Preparation process for extracting, separating and purifying picroside I and picroside II from Picrorrhiza Kurrooa Royleex Benth |
| CN104693253A (en) * | 2015-03-30 | 2015-06-10 | 济南东源生物医药技术有限公司 | Industrial preparation method for high-purity 6'-O-trans-cinnamyl catalpol |
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