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Method for preparing molecularly imprinted polymers of ethinylestradiol analogue

A technology of molecular imprinting and polymer, which is applied in the field of preparation of enrichment and separation materials, can solve the problems of false positive results, elution of template molecules, leakage, etc.

Inactive Publication Date: 2011-01-26
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current molecular imprinting technology for estradiol uses polymers to detect template molecules. Since it is impossible to elute all template molecules during elution, it will cause "leakage" and result in false positives.

Method used

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  • Method for preparing molecularly imprinted polymers of ethinylestradiol analogue
  • Method for preparing molecularly imprinted polymers of ethinylestradiol analogue
  • Method for preparing molecularly imprinted polymers of ethinylestradiol analogue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 2.96g (1mmol) ethinyl estradiol solid powder is dissolved in the eggplant-shaped bottle that the ethanol solution of 15mL is housed, adds a small amount of Pd / C, feeds hydrogen under the normal temperature in the electromagnetic stirring, high-efficiency liquid phase tracking reaction process (detection wavelength is 280nm, the mobile phase is methanol-water with a volume ratio of 8:2, and the flow rate is 1mL / min), until the peak of ethinyl estradiol cannot be detected, indicating that the reaction is complete. Filter out Pd / C, spin dry ethanol, add appropriate amount of ethanol for recrystallization, and obtain colorless needle crystals.

[0019] 1 H-NMR (CDCl 3 )δ: 0.92(s, 3H, 18-CH 3 ), 1.03(t, 3H, CH 2 CH 3 ), 2.82 (m, 2H, 6-CH 2 ), 4.61(b, 2H, OH-phenol), 6.56(d, 1H, 4-CH), 6.63(d, 1H, 2-CH), 7.15(d, 1H, 1-CH).M / z: 283.2([M-H 2 O] + , 100%).

Embodiment 2

[0021] Dissolve 0.25 mmol of the nominal template 17-ethylestradiol and 0.25 mmol of the functional monomer methacrylic acid into 15 mL containing 1 mmol of the crosslinker trimethylolpropane trimethacrylate, 20 mg of the initiator azobisiso In the acetonitrile solution of butyronitrile, ultrasonication, nitrogen gas for 10min, sealing, precipitation polymerization in oil bath at 60°C for 12h to generate white powdery polymer, use methanol-acetic acid solution with a volume ratio of 9:1 as the extraction solution to remove template molecules until Until the template molecule cannot be detected by the ultraviolet detector, then wash and centrifuge with methanol at a centrifugation speed of 15000rpm, discard the supernatant, and dry the polymer in a vacuum oven at 40°C to a constant weight to obtain the ethinyl estradiol analog molecule Imprinted polymer.

Embodiment 3

[0023] Dissolve 0.25 mmol of the nominal template 17-ethylestradiol and 0.25 mmol of the functional monomer methacrylic acid into 15 mL containing 1 mmol of the crosslinker trimethylolpropane trimethacrylate, 20 mg of the initiator azobisiso In the acetonitrile solution of butyronitrile, ultrasonication, nitrogen gas for 10 minutes, sealing, precipitation polymerization in 60 ° C oil bath for 16 hours to form a white powdery polymer, use methanol-acetic acid solution with a volume ratio of 9:1 as the extraction solution to remove template molecules until Until the template molecule cannot be detected by the ultraviolet detector, then wash and centrifuge with methanol at a centrifugation speed of 15000rpm, discard the supernatant, and dry the polymer in a vacuum oven at 40°C to a constant weight to obtain the ethinyl estradiol analog molecule Imprinted polymer.

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Abstract

The invention relates to a method for preparing molecularly imprinted polymers of ethinylestradiol analogue. The method comprises the following preparation steps: a, taking 17-ethenyl estradiol as a template, mixing template molecules, functional monomers, a crosslinking agent, a pore-foaming agent and an initiator, performing ultrasonic polymerization on the mixture for 12 to 24 hours at the temperature of 60 DEG C in the atmosphere of nitrogen, and obtaining polymers; b, performing centrifugation on the prepared polymers, discarding supernatant, using a methanol-acetic acid mixture for soakcleaning and removal of the template molecules, and obtaining the molecularly imprinted polymers; and c, performing vacuum drying on the polymers. Because the template is easy to separate from ethinylestradiol and estradiol on a chromatographic column, the prepared MIP cannot influence the accuracy of a result due to the leakage of the template when being used for solid-phase extractive materials.Moreover, the prepared MIP reveals obvious compatibility to the 17-ethenyl estradiol, the ethinylestradiol and the estradiol, and corresponding non-imprinted polymers (polymers prepared without the template in the same condition) reveal low compatibility.

Description

1. Technical field [0001] The invention belongs to molecular imprinted polymer preparation technology, in particular to a method for preparing enrichment and separation materials with high selectivity and high affinity for steroid hormone drugs such as ethinyl estradiol and estradiol. 2. Background technology [0002] Steroid hormones that may remain in the environment or animal foods are potentially harmful to people's health and have become an important proposition in the field of food safety. Such as estradiol, ethinylestradiol (17α-ethinylestradiol, EE2), etc., their activity is obviously stronger than natural steroid hormones, so they are widely used in the synthesis of contraceptives and the treatment of diseases in medicine, and also in livestock, aquaculture As a growth promoter in animals. These hormonal substances are often excreted into the environment in the form of drug prototypes or metabolites with feces, urine and other excrements. Most hormonal drugs are st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F220/06C08F2/44C08J9/26C08F220/56C08F220/28C08F220/14
Inventor 李飞殷晓佳江珂彭艳都述虎胡琴周学敏
Owner NANJING MEDICAL UNIV