Unlock instant, AI-driven research and patent intelligence for your innovation.

Separation and purification method of notopterol monomer

A technology for separation and purification, Qiang live alcohol, applied in the direction of organic chemistry, etc., can solve the problems of waste of reagents, low product yield, long production cycle, etc., and achieve the effect of improving the concentration of the target substance, improving the separation effect, and reducing energy consumption.

Active Publication Date: 2015-04-08
CHENGDU PUSH BIOLOGICAL TECH
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] According to related searches, the purification of notopterythyl alcohol monomer mainly adopts conventional column chromatography, that is, the method of combining silica gel column chromatography and crystallization, which has a long production cycle, serious waste of reagents, and low product yield.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Separation and purification method of notopterol monomer
  • Separation and purification method of notopterol monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for separating and purifying notopterythyl alcohol monomer, comprising the following process steps:

[0035] 1) extract

[0036] Crush 1 kg of Notopterygium medicinal material into a coarse powder of 1-4 mm, add 10 L of methanol solution with a concentration of 90% by volume, extract 3 times, each time for 2 hours, recover methanol, and combine the filtrate, a total of 2.9 L;

[0037] 2) Extraction

[0038] The filtrate obtained in step 1) was added to an equal volume of ethyl acetate to extract 3 times, and the upper layer solution was separated and concentrated to dryness to obtain 80 g of solids;

[0039] 3) Dissolving filtration

[0040] Step 2) Add 400mL of methanol to dissolve the obtained solid, filter the solution to obtain 400mL of filtrate;

[0041] 4) HPLC preparation

[0042] The filler is C 18 chromatographic column, the column specification is 50cm×8cm;

[0043] The composition of the mobile phase is: acetonitrile-water solution (50:50)

[...

Embodiment 2

[0053] A method for separating and purifying notopterythyl alcohol monomer, comprising the following process steps:

[0054] 1) extract

[0055] Crush 10 kg of notopterygium medicinal materials into a coarse powder of 1-4 mm, add 90 L of methanol solution with a concentration of 95% by volume, extract 4 times, each time for 3 hours, recover methanol, and combine the filtrate, a total of 18 L;

[0056] 2) extraction

[0057] The filtrate obtained in step 1) was added into an equal volume of ethyl acetate to extract 4 times, and the upper layer solution was separated and concentrated to dryness to obtain 85 g of solid matter;

[0058] 3) Dissolving and filtering

[0059] Step 2) Add 680mL of methanol to dissolve the obtained solid, filter the solution to obtain 680mL of filtrate;

[0060] 4) HPLC preparation

[0061] The filler is C 18chromatographic column, the column specification is 50cm×10cm;

[0062] The composition of the mobile phase is: acetonitrile-water solution ...

Embodiment 3

[0072] A method for separating and purifying notopterythyl alcohol monomer, comprising the following process steps:

[0073] 1) extract

[0074] Crush 50 kg of notopterygium medicinal materials into a coarse powder of 1-4 mm, add 300 L of methanol solution with a concentration of 80% by volume, extract 3 times, each time for 2 hours, recover methanol, and combine the filtrate, a total of 125 L;

[0075] 2) extraction

[0076] The filtrate obtained in step 1) was added to an equal volume of ethyl acetate to extract 3 times, and the upper layer solution was separated and concentrated to dryness to obtain 410 g of solids;

[0077] 3) Dissolving and filtering

[0078] Step 2) Add 2460mL of methanol to dissolve the obtained solid, filter the solution to obtain 2460mL of filtrate;

[0079] 4) HPLC preparation

[0080] The filler is C 18 chromatographic column, the column specification is 50cm×15cm;

[0081] The composition of the mobile phase is: acetonitrile-water solution (5...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a separation and purification method of a notopterol monomer, and belongs to the technical field of traditional Chinese medicines. The separation and purification method comprises the following steps in sequence: based on root stocks of umbelliferae notopterygium root as raw materials, carrying out ethanol solution extraction, ethyl acetate extraction, methanol dissolution and filtration, high-performance preparative liquid chromatography separation and product recycling to obtain the notopterol monomer. According to the preparation method, the optimal technology and parameter conditions are utilized, thus the content of the notopterol in the notopterol monomer is up to more than 98%; and the method is stable in the whole technological process, simple and convenient for operation, high in separating efficiency and low in cost, can realize high-purity separation and preparation of the notopterol monomer as mass.

Description

technical field [0001] The invention relates to a preparation method of a plant compound monomer, in particular to a separation and purification method for extracting notopterygium alcohol monomer from notopterygium, and belongs to the technical field of traditional Chinese medicine. Background technique [0002] Notopterygium (Rhizoma et Radix Notopterygii) is the dried rhizome and root of Notopterygium incisum Ting ex H. T. Chang or Notopterygium forbesii Boiss. of Umbelliferae. Notopterygium active warm taste bitter, pungent, into the bladder, kidney meridian. It has the effects of dispelling exterior cold, removing rheumatism, and sharpening joints. Treatment of exogenous wind-cold, headache without sweating, wind-cold-damp arthralgia, strong neck and tendons, aching joints, feng shui edema, pain, swelling and sores. [0003] Notopterol is also called Notopterol, incised Notopterygium, and its molecular formula is C 21 h 22 o 5 , the molecular weight is 354.40, and ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
Inventor 白兰辉夏柯文焕松陈军钟钰刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH