CN106220695A - A kind of industrial production process of catalpol - Google Patents
A kind of industrial production process of catalpol Download PDFInfo
- Publication number
- CN106220695A CN106220695A CN201610579749.5A CN201610579749A CN106220695A CN 106220695 A CN106220695 A CN 106220695A CN 201610579749 A CN201610579749 A CN 201610579749A CN 106220695 A CN106220695 A CN 106220695A
- Authority
- CN
- China
- Prior art keywords
- catalpol
- production process
- industrial production
- radix rehmanniae
- filtrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The invention discloses the industrial production process of a kind of catalpol, belong to medicine, chemical technology field, China's plant resources containing catalpol is the abundantest, particularly in Radix Rehmanniae, catalpol content is the highest, catalpol content in domestic report Radix Rehmanniae is a times of Radix Rehmanniae, during Processing methods, contained catalpol declines to a great extent and even disappears, for this, the present invention is that Radix Rehmanniae opens up a feasible road through Processing methods, the raw material used is Radix Rehmanniae, the problem solving catalpol content loss, and technique is simple, solve industrialized production problem, purity reaches highly purified crude drug rank simultaneously, the problem solving industrialized production.
Description
Technical field
The present invention relates to the industrial production process of a kind of catalpol, belong to medicine, chemical technology field.
Background technology
Catalpol (Catalpol) is derived from the fresh rhizome that Radix Rehmanniae is scrophulariaceae rehmannia glutinosa plant.China plants containing catalpol
Goods and materials source is the abundantest, particularly high-load plant, if Radix Rehmanniae is the large medicinal herbs most in use of China, provides for catalpol new drug development
Resource Guarantee, in Radix Rehmanniae, catalpol content is the highest, and during Processing methods, contained catalpol declines to a great extent and even disappears.To this end, this
Invention is the Radix Rehmanniae inherent mechanism that the property of medicine changes through Processing methods, opens up a feasible road.The present invention uses
Raw material be Radix Rehmanniae, the problem solving catalpol content loss, and technique is simple, solves industrialized production problem, simultaneously
Purity reaches the crude drug rank of more than 98%.Catalpol has anticancer, neuroprotective, antiinflammatory, diuresis, blood sugar lowering and hepatitis virus resisting
Deng effect.
Summary of the invention
It is an object of the invention to provide the industrial production process of a kind of catalpol, with solve cannot industrialization and purity higher
Problem.To achieve these goals, the present invention uses Radix Rehmanniae to be raw material, obtains filtrate, use volume ratio after size-reduced squeezing
For the methanol of 1:10, precipitate with ethanol 24h, after cryoconcentration, obtain colloid substance, be dissolved in water through resin column, 70% ethanol elution, TLC
Tracing detection collects object, cryoconcentration, 5% aqueous acetonitrile solution, utilizes preparation liquid phase again to separate, is concentrated to give crude product Chinese catalpa
Alcohol, obtains sterling after recrystallization.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described employing Radix Rehmanniae is raw material, size-reduced squeezing
After obtain filtrate, the most singly refer to use Radix Rehmanniae be raw material, obtain filtrate after size-reduced squeezing, also include that Radix Rehmanniae directly squeezes
Filtrate.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described volume ratio is the methanol of 1:10, the most singly refers to
Its volume ratio is the methanol of 1:10, also includes 1:5-1:15.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described precipitate with ethanol 24h, the most singly refer to precipitate with ethanol 24h, also wrap
Include 12h-30h.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: after described cryoconcentration, obtain colloid substance, its glue
Shape material proportion is 1.4-1.6.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that be dissolved in water described in: through resin column, its resin column type
Number it is XDA-7.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described TLC tracking and monitoring collects object, its exhibition
Opening agent is chloroform: methanol: water=14:7:1, and color condition is 10% ethanol solution of sulfuric acid.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described 70% ethanol elution, the most singly refer to 70% ethanol
Eluting, also includes 10% eluting impurity, collects 50%-80% eluent.
The industrial production process of above-mentioned a kind of catalpol, it is characterised in that: described utilization preparation liquid phase separates again, its eluting
Condition is 5% acetonitrile isocratic elution, and detection wavelength is 270nm.
Catalpol structural formula is as follows:
Detailed description of the invention
Embodiment:
The industrial production process of described a kind of catalpol: taking 5Kg Radix Rehmanniae is raw material, obtains filtrate 4Kg after size-reduced squeezing,
Adding 20Kg methanol, precipitate with ethanol filters the most afterwards, after 80 DEG C of cryoconcentration of filtrate, obtains colloid substance, uses 1L water dissolution, through XDA-7 tree
Fat post, 10% ethanol elution impurity, 70% ethanol elution collects object, TLC tracing detection, 80 DEG C of cryoconcentration to without alcohol,
Again by 5% aqueous acetonitrile solution, preparation liquid phase is utilized again to separate, 5% acetonitrile eluting, collect object, be concentrated to give crude product catalpol
56g, recrystallization obtains sterling 35g.
Accompanying drawing explanation
Fig. 1 is the present invention final sterling IR collection of illustrative plates.
Fig. 2 is the present invention final sterling HPLC collection of illustrative plates.
Claims (8)
1. an industrial production process for catalpol, the present invention uses Radix Rehmanniae to be raw material, obtains filtrate, use body after size-reduced squeezing
The long-pending ratio methanol for 1:10, after precipitate with ethanol, cryoconcentration, obtains colloid substance, with water dissolution through resin column, and 70% ethanol elution, TLC
Tracing detection collects object, by 5% aqueous acetonitrile solution after concentration, utilizes preparation liquid phase again to separate, is concentrated to give crude product catalpol,
Sterling is obtained after recrystallization.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that: described employing Radix Rehmanniae is raw material, warp
Obtain filtrate after pulverizing squeezing, the most singly refer to that using Radix Rehmanniae is raw material, obtains filtrate after size-reduced squeezing, also includes that Radix Rehmanniae is straight
Connect and squeeze to obtain filtrate.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that: described volume ratio is the first of 1:10
Alcohol, Dan Zhiqi volume ratio is not the methanol of 1:10, also includes 1:5-1:15.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that: after described cryoconcentration, obtain jelly
Matter, its colloid substance proportion is 1.4-1.6.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that be dissolved in water described in: through resin column, its
Resin column model is XDA-7.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that: described 70% ethanol elution, the most singly refer to
70% ethanol elution, also includes 10% eluting impurity, collects 50%-80% eluent.
The industrial production process of a kind of catalpol the most as claimed in claim, it is characterised in that: described utilization preparation liquid phase is divided again
From, its elution requirement is 5% acetonitrile isocratic elution, and detection wavelength is 270nm.
The industrial production process of a kind of catalpol the most as claimed in claim: taking 5Kg Radix Rehmanniae is raw material, obtains after size-reduced squeezing
Filtrate 4Kg, adds 20Kg methanol, and precipitate with ethanol filters the most afterwards, after 80 DEG C of cryoconcentration of filtrate, obtains colloid substance, uses 1L water dissolution, warp
XDA-7 resin column, 10% ethanol elution impurity, 70% ethanol elution collects object, TLC tracing detection, 80 DEG C of cryoconcentration
Extremely without alcohol, then by 5% aqueous acetonitrile solution, preparation liquid phase is utilized again to separate, 5% acetonitrile eluting, collect object, be concentrated to give thick
Product catalpol 56g, recrystallization obtains sterling 35g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610579749.5A CN106220695A (en) | 2016-07-21 | 2016-07-21 | A kind of industrial production process of catalpol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610579749.5A CN106220695A (en) | 2016-07-21 | 2016-07-21 | A kind of industrial production process of catalpol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106220695A true CN106220695A (en) | 2016-12-14 |
Family
ID=57531200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610579749.5A Pending CN106220695A (en) | 2016-07-21 | 2016-07-21 | A kind of industrial production process of catalpol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106220695A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265282A (en) * | 2008-05-05 | 2008-09-17 | 山东大学 | Method for separating catalpol from fresh rehmanniae root |
| CN102058712A (en) * | 2009-11-13 | 2011-05-18 | 上海玉森新药开发有限公司 | Rehmannia stem and leaf extract and preparation method and application thereof |
| CN102863489A (en) * | 2011-07-04 | 2013-01-09 | 苏州玉森新药开发有限公司 | Method for extracting catalpol from rehmannia stem |
-
2016
- 2016-07-21 CN CN201610579749.5A patent/CN106220695A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265282A (en) * | 2008-05-05 | 2008-09-17 | 山东大学 | Method for separating catalpol from fresh rehmanniae root |
| CN102058712A (en) * | 2009-11-13 | 2011-05-18 | 上海玉森新药开发有限公司 | Rehmannia stem and leaf extract and preparation method and application thereof |
| CN102863489A (en) * | 2011-07-04 | 2013-01-09 | 苏州玉森新药开发有限公司 | Method for extracting catalpol from rehmannia stem |
Non-Patent Citations (1)
| Title |
|---|
| 杨洪枫等，: "地黄中梓醇的研究进展", 《亚太传统医药》 * |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161214 |