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Preparation method of molecularly imprinted polymer of methyltestosterone

A technology of methyltestosterone and molecular imprinting, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of large loss, large specific surface area of ​​molecularly imprinted polymers, and uneven particle size of polymers, so as to save costs, Good recognition ability and selection characteristics, the effect of overcoming uneven particle size

Inactive Publication Date: 2011-01-12
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing methyltestosterone molecularly imprinted polymers, which has the advantages of simple operation, easy process control, and low cost; overcomes the disadvantages of uneven particle size and large loss of the obtained polymer, and obtains The molecularly imprinted polymer has a large specific surface area and can be used directly without grinding and sieving

Method used

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  • Preparation method of molecularly imprinted polymer of methyltestosterone
  • Preparation method of molecularly imprinted polymer of methyltestosterone
  • Preparation method of molecularly imprinted polymer of methyltestosterone

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Embodiment 1

[0046] A method for preparing a methyltestosterone molecularly imprinted polymer, comprising the steps of:

[0047] (1) Dissolving the template molecule methyltestosterone in the porogen acetonitrile at a ratio of about 60ml / mmol, then mixing it with the polymerized monomer methacrylic acid (MAA) at a ratio of 1:3, and shaking for 2 hours;

[0048] (2) Add cross-linking agent ethylene glycol dimethacrylate and initiator azobisisobutyronitrile (AIBN) to the product of step (1), mix well; dissolve the dispersant polyvinyl alcohol in 80°C water, the aqueous solution was added dropwise to the above mixed solution, and N 2 10min to remove O 2 , sealed and placed in a water bath at 60°C, stirred for 18 hours at the same time, solid-liquid separation, and the solid phase part was taken after high-speed centrifugation; wherein, the ratio of cross-linking agent to methyltestosterone was 1:20, and the ratio of initiator to methyltestosterone was 70mg / mmol, the ratio of dispersant to ...

Embodiment 2

[0057] (1) Dissolving the template molecule methyltestosterone in the porogen methanol at a ratio of about 6ml / mmol, then mixing it with the polymerized monomer acrylamide (AA) at a ratio of 1:8, and shaking for 4 hours;

[0058] (2) Add crosslinking agent trimethoxypropane trimethacrylate and initiator azobisisoheptanonitrile (ABVN) to the product of step (1), mix well; dissolve dispersant polystyrene in 100°C In the water, the aqueous solution was added dropwise to the above mixed solution, and argon was passed through for 10 minutes to remove O 2 Wait for oxygen-containing gas, seal and place in a water bath at 55°C, stir for 24 hours at the same time, separate solid and liquid, and take the solid phase part after high-speed centrifugation; wherein, the ratio of crosslinking agent to methyltestosterone is 1:30, and the ratio of initiator to methyltestosterone is 1:30. The ratio of testosterone is 40mg / mmol, and the ratio of dispersant to methyltestosterone is 5g / mmol.

[0...

Embodiment 3

[0064] (1) Dissolving the template molecule methyltestosterone in the porogen acetone at a ratio of about 30ml / mmol, then mixing it with the polymerized monomer trifluoromethacrylic acid (TFMAA) at a ratio of 1:5, and shaking for 0.5h;

[0065] (2) Add cross-linking agent and initiator azobisisobutyronitrile (AIBN) to the product of step (1), and mix well; dissolve the dispersant polystyrene in water at 90°C, and add the aqueous solution dropwise Into the above mixed solution, pass N 2 10min to remove O 2 Wait for oxygen-containing gas, seal it in a water bath at 65°C, stir for 30 hours at the same time, separate the solid from the liquid, and take the solid phase part after high-speed centrifugation; among them, the crosslinking agent is ethylene glycol dimethacrylate and trimethoxypropane trimethacrylate The mixture of methacrylate, the ratio of cross-linking agent and methyl testosterone is 1:10, the ratio of initiator and methyl testosterone is 100 mg / mmol, and the ratio ...

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Abstract

The invention relates to a preparation method of a molecularly imprinted polymer of methyltestosterone, and the preparation method comprises the following steps: dissolving the methyltestosterone into a pore-forming agent with the proportion of 6-60ml / mmol, then mixing with a polymerized monomer according to the proportion of 1:3-1:8, and oscillating for 0.5-4h; adding a cross-linking agent and an initiator, uniformly mixing, adding water solution of dispersant into the mixed solution dropwise, introducing inert gas for 10-20min, sealing and placing in a water bath at 55-65 DEG C, simultaneously stirring for 18-30h, carrying out solid-liquid separation and taking the solid phase part; and extracting with an acid organic solvent, further extracting with a pure organic solvent and obtaining a product. The method has the advantages of simple operation, easy control of the process, low cost and the like, and can overcome the shortcomings of non-uniform particle size of the obtained polymer, great loss and the like; and the obtained molecularly imprinted polymer has large specific surface area and can be directly used without grinding and screening.

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 suspension 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 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 regulations. To compl...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F220/56C08F220/04C08F2/44C08F2/20C08J9/26B01J20/26B01J20/30
Inventor 杨敏莉沈蕊莲储晓刚王大宁
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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