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A double-template molecular imprinting purification method for tetrandrine A and B

A technology of molecular imprinting and purification method, which is applied in the field of tetrandrine and tetrandrine, can solve the problems of cumbersome purification steps and achieve the effects of improving safety, promoting development and application, and high loss

Active Publication Date: 2022-05-17
CSPC JIANGXI GOLDEN LOTUS PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, due to the similar structural properties of tetrandrine and B, in the process of purifying by single-molecule imprinting, it is inevitable that there will be interspersion of mutual components, resulting in the need for further purification after purification by single-molecule imprinting, making the purification step It is more cumbersome, which limits the application of molecular imprinting in the purification of A and B from Tetrandine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A double-template molecular imprinted purification method for tetrandrine A and B comprises the following steps:

[0028] 1) Preparation of double-template molecularly imprinted polymer: Weigh 40 mmol of tetrandrine and B, mix with 160 mmol of methacrylic acid, place in a stoppered Erlenmeyer flask, and use a mixed solvent of toluene and acetonitrile at a volume ratio of 1:1 Dissolve, seal, and vibrate in a shaker for 4 hours to fully react; add 800mmol ethylene glycol dimethacrylate and 480mmol azobisisobutylcyanide, shake well, transfer the solution into a glass ampoule, and blow nitrogen for 20 minutes to remove Oxygen; react in a constant temperature water bath at 60°C for 40 hours; filter the generated polymer to remove the solvent, cool to room temperature, grind, and pass through a 100-mesh sieve; pack the sieved polymer into a column, and use 70% ethanol aqueous solution to elute the template molecules and untreated polymers. Reaction or excess functional monome...

Embodiment 2

[0032] A double-template molecular imprinted purification method for tetrandrine A and B comprises the following steps:

[0033] 1) Preparation of double-template molecularly imprinted polymer: Weigh 40 mmol of tetrandrine and B, mix with 120 mmol of methacrylic acid, place in a stoppered Erlenmeyer flask, and use a mixed solvent of toluene and acetonitrile at a volume ratio of 1:5 Dissolve, seal, shake in a shaker for 1 hour to fully react; add 1000mmol ethylene glycol dimethacrylate and 600mmol azobisisobutylcyanide, shake well, transfer the solution into a glass ampoule, blow nitrogen for 5 minutes to remove Oxygen; react in a constant temperature water bath at 40°C for 48 hours; filter the generated polymer to remove the solvent, cool to room temperature, grind, and pass through a 50-mesh sieve; pack the sieved polymer into a column, and use 50% ethanol aqueous solution to elute the template molecules and untreated polymers. Reactive or excess functional monomers, the elut...

Embodiment 3

[0037] A double-template molecular imprinted purification method for tetrandrine A and B comprises the following steps:

[0038] 1) Preparation of double-template molecularly imprinted polymer: weigh 40 mmol of tetrandrine and B, mix with 200 mmol of methacrylic acid, place in a stoppered Erlenmeyer flask, use a mixed solvent of toluene and acetonitrile with a volume ratio of 1:3 Dissolve, seal, and vibrate in a shaker for 2 hours to fully react; add 600mmol ethylene glycol dimethacrylate and 400mmol azobisisobutylcyanide, shake well, transfer the solution into a glass ampoule, and blow nitrogen for 15 minutes to remove Oxygen; react in a constant temperature water bath at 50°C for 30 hours; filter the generated polymer to remove the solvent, cool to room temperature, grind, and pass through a 100-mesh sieve; pack the sieved polymer into a column, and use 80% ethanol aqueous solution to elute the template molecules and untreated polymers. Reaction or excess functional monomers...

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Abstract

The present invention relates to a medicine extraction and purification technology, in particular, it provides a technical method for efficiently separating tetrandrine and B at the same time; that is, using methacrylic acid, ethylene glycol dimethacrylate and azobis Isobutylcyanide and other target molecular powders tetrandrine and B are synthesized, and then the target molecule is eluted to obtain a double-template molecularly imprinted polymer. The column and preparative chromatograph further separate the tetrandrine and B, and the purity of the obtained tetrandrine and B reaches more than 99%.

Description

technical field [0001] The invention relates to a technology for extracting and purifying raw materials of natural medicines, in particular to a technology for simultaneously purifying tetrandrine and tetrandrine B in powdered tetrandrine by using double-template molecular imprinting. Background technique [0002] Fenfangji, also known as Hanfangji and Baimuxiang, is the root of the plant Fangji in the family Fangjiaceae. Tetrandrine, also known as tetrandrine, also known as tetrandrine and tetrandrine, is an antihypertensive drug and is mainly used clinically to treat mild and moderate hypertension, and can also be used for hypertensive crisis. Tetanin has anti-inflammatory, analgesic, antihypertensive and anti-tumor effects. [0003] With the deepening of people's understanding of tetrandrine and its active ingredients, tetrandrine and tetrandrine have been used more and more; at present, the method of solvent reflux or percolation is mainly used to extract tetrandrine an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/18B01D15/08B01J20/26B01J20/30C08F222/14C08F220/06C08J9/28
CPCC07D491/18C08F222/1006C08J9/28B01D15/08B01J20/268C08J2201/0502C08J2335/02
Inventor 陈金龙黄文超黄丽莉揭建林朱培林杨燕欢郜杰康月菊
Owner CSPC JIANGXI GOLDEN LOTUS PHARMA CO LTD
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