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Method for preparing methyltestosterone molecularly-imprinted polymer

A technology of methyltestosterone and molecular imprinting, which is applied in the field of precipitation polymerization preparation of methyltestosterone molecularly imprinted polymers, can solve the problems that the preparation method of methyltestosterone has not been reported yet, achieve good recognition ability and selection characteristics, and the process is easy Effects of control, good binding and dissociation

Inactive Publication Date: 2011-02-02
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are no reports about methyltestosterone molecularly imprinted polymers and their preparation methods

Method used

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  • Method for preparing methyltestosterone molecularly-imprinted polymer
  • Method for preparing methyltestosterone molecularly-imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A method for preparing a methyltestosterone molecularly imprinted polymer, the preparation method comprising the steps of:

[0044] (1) Add the template molecule methyltestosterone and the polymerized monomer methacrylic acid (MAA) in a ratio of 1:5 to the porogen acetonitrile whose ratio to methyltestosterone is 50ml / mmol, and stir at 2°C for 3h ;

[0045] (2) Add cross-linking agent ethylene glycol dimethacrylate (EDMA) and initiator azobisisobutyronitrile (AIBN) in the product of step (1), then add the ratio with methyltestosterone to be 450ml / 1 mmol of porogen acetonitrile was thermally initiated at 60°C for 20 hours, and precipitated by high-speed centrifugation; wherein, the ratio of cross-linking agent ethylene glycol dimethacrylate (EDMA) to methyl testosterone was 1:20, and the initiator The ratio of azobisisobutyronitrile (AIBN) to methyltestosterone is 70mg / mmol.

[0046] (3) The precipitate in step (2) was extracted with a mixed solution of methanol and a...

Embodiment 2

[0051] A method for preparing a methyltestosterone molecularly imprinted polymer, the preparation method comprising the steps of:

[0052] (1) Add the template molecule methyltestosterone and the polymerized monomer acrylamide (AA) in a ratio of 1:3 to the porogen methanol whose ratio to methyltestosterone is 500ml / mmol, and stir at 8°C for 0.5h ;

[0053] (2) Add crosslinking agent trimethoxypropane trimethacrylate (TRIM) and initiator azobisisoheptanonitrile (ABVN) to the product of step (1), thermally initiate polymerization at 65°C for 16h, and High-speed centrifugation obtains precipitation; Wherein, the ratio of cross-linking agent ethylene glycol dimethacrylate (EDMA) and methyl testosterone is 1: 10, and the ratio of initiator azobisisoheptanonitrile (ABVN) and methyl testosterone is 40mg / mmol.

[0054] (3) The precipitate in step (2) was extracted with a mixed solution of methanol and trifluoroacetic acid for 12 hours to remove template molecules, and then extracte...

Embodiment 3

[0059] A method for preparing a methyltestosterone molecularly imprinted polymer, the preparation method comprising the steps of:

[0060] (1) Add the template molecule methyltestosterone and trifluoromethacrylic acid (TFMAA) in a ratio of 1:8 to the porogen acetone whose ratio to methyltestosterone is 300ml / mmol, and stir at 5°C for 1.5h ;

[0061] (2) Add cross-linking agent and initiator azobisisoheptanonitrile (ABVN) to the product of step (1), thermally initiate polymerization at 50° C. for 24 hours, and obtain a precipitate through high-speed centrifugation; wherein, the cross-linking agent is B A mixture of diol dimethacrylate (EDMA) and trimethoxypropane trimethacrylate (TRIM), the ratio of methyl testosterone to 1:30, the initiator azobisisoheptanonitrile (ABVN) and methyl The ratio of testosterone is 100 mg / mmol.

[0062] (3) The precipitate in step (2) was extracted with a mixed solution of methanol and formic acid for 24 hours to remove template molecules, and th...

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Abstract

The invention discloses a method for preparing a methyltestosterone molecularly-imprinted polymer, in particular a precipitation polymerization preparation method for the methyltestosterone molecularly-imprinted polymer. The preparation method comprises the following steps of: adding methyltestosterone and polymerization monomer in a ratio of 1:3-1:8 into a pore-forming agent, and stirring the mixture for 0.5 to 3 hours at a low temperature; then adding a cross linker and an initiator into the mixture, performing thermal initiated polymerization, centrifuging the solution at a high speed, and then taking sediment; and extracting the sediment by an acid organic solvent to remove template molecules, then extracting the sediment by using an organic solvent to remove the residual acid substances, and drying the sediment in vacuum to obtain a product. The method has the advantages of simple operation, good repeatability, easy control of processes and the like; the obtained molecularly-imprinted polymer has controllable particle diameter and uniform size; and the polymer has good identification capability and selection property on the methyltestosterone, and has good bonding capability and separating capability.

Description

technical field [0001] The invention relates to a method for preparing a methyltestosterone molecularly imprinted polymer, in particular to a method for preparing a methyltestosterone molecularly imprinted polymer by precipitation polymerization. Background technique [0002] Methyltestosterone is a synthetic metabolic steroid, as a growth-stimulating agent, it has been widely used in animal husbandry and aquatic products in the last century. However, due to the slow metabolism and strong accumulation of methyltestosterone, it will enter the human body through the food chain and cause serious toxic and side effects, such as: liver poisoning, carcinotoxicity, and carcinogenicity. The European Union banned the use of steroid hormones such as methyltestosterone in livestock as early as 1988. In my country, since 1999, the use of methyltestosterone as a growth-promoting agent has been banned by law. But so far, there are still a few companies using it in violation of regulatio...

Claims

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Application Information

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IPC IPC(8): C08F220/56C08F220/06C08F2/44C08F220/04C08F220/28C08K5/07C08F222/14C08J9/26
Inventor 杨敏莉沈蕊莲储晓刚王大宁
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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