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Method for producing molecular engram polyalcohol microsphere and method for separating enrofloxacin thereof

A molecular imprinting and enrofloxacin technology, applied in chemical analysis, analytical materials, instruments, etc., can solve the problems of irregular particle shape, low yield, molecular recognition and selectivity decline of molecularly imprinted polymers, etc. The effect of high selectivity and sensitivity, strong recognition ability

Inactive Publication Date: 2010-03-24
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Novel enrofloxacin imprinted polymer applied to the solid-phase extraction of fluorinated quinolones from urine and tissue samples" published in "Analytica Chimica Acta" (2006, 562, 145-151) by Ester Caro et al. Star) proposed that the combination of molecularly imprinted polymers and HPLC detection methods can increase the detection sensitivity of enrofloxacin to 50 μg / kg; Molecularly imprinted polymer particles with large diameters, and they have the disadvantages of low yield, irregular particle shape, poor dispersion, etc., and the molecular recognition and selectivity of molecularly imprinted polymers will decrease during the grinding process, and the product cannot be directly obtained from aqueous solution. Extract the analyte

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Preparation of molecularly imprinted polymer microspheres of enrofloxacin:

[0034] (1) The mol ratio of enrofloxacin, functional monomer and ethylene glycol dimethacrylate is 1: 4: 25; The volume ratio of the total volume of chloroform and ethylene glycol dimethacrylate to water is 1 : 8; the concentration of polyvinyl alcohol 1788 (PVA1788) is 3%; 0.339ml functional monomer methacrylic acid and 1mmol enrofloxacin are dissolved in chloroform, and ultrasonication is performed for 5~10min; 5ml ethylene glycol dimethyl Acrylate, 120mg of azobisisobutyronitrile and 15ml of chloroform were mixed, and ultrasonication was applied for 5 to 10 minutes;

[0035] Mix the above three solutions, 60-70°C water bath, 400-500rpm, keep nitrogen atmosphere and stir for 24h; (2) After the reaction, stir in 70°C water for 60min, filter, wash twice with 50ml double distilled water, 50ml methanol Wash 3 times, wash 2 times with 50ml acetone (to remove residual dispersant, monomer and ot...

Embodiment 2

[0046] 1. Preparation of molecularly imprinted polymer microspheres of enrofloxacin:

[0047] (1) The molar ratio of template molecule, functional monomer and ethylene glycol dimethacrylate is 0.5:4:25; the volume ratio of the total volume of chloroform and ethylene glycol dimethacrylate to water is 1:5 ; The concentration of polyvinyl alcohol 1788 (PVA1788) is 4%; 0.339ml of functional monomer methyl methacrylate and 0.5mmol of enrofloxacin are dissolved in chloroform, and ultrasonically applied for 5-10min; 5ml of ethylene glycol dimethyl Acrylic acid ester, 120mg of azobisisobutyronitrile and 15ml of chloroform were mixed, and ultrasonically applied for 5 to 10 minutes; the above three solutions were mixed, in a water bath at 60 to 70°C, at 400 to 500 rpm, and stirred for 24 hours in a nitrogen atmosphere; (2) the reaction was completed Afterwards, stir in 70°C water for 60 minutes, filter, wash with 50ml double-distilled water twice, 50ml methanol three times, and 50ml ace...

Embodiment 3

[0054] 1. Preparation of molecularly imprinted polymer microspheres of enrofloxacin:

[0055] (1) The molar ratio of template molecule, functional monomer and ethylene glycol dimethacrylate is 0.33:4:25; the volume ratio of the total volume of chloroform and ethylene glycol dimethacrylate to water is 1:6 The concentration of polyvinyl alcohol 1788 (PVA1788) is 5%; 0.339ml functional monomer N-diethylaminoethyl ester or 4-vinylpyridine or methacrylic acid N and 0.33mmol enrofloxacin are dissolved in chloroform, Ultrasound for 5-10 minutes; mix 5ml ethylene glycol dimethacrylate, 120mg azobisisobutyronitrile and 15ml chloroform, and apply ultrasound for 5-10 minutes; mix the above three solutions, put them in a water bath at 60-70℃, and set them in a 400- 500rpm, keep stirring under nitrogen atmosphere for 24h; (2) After the reaction, stir in 70°C water for 60min, filter, wash with 50ml double distilled water twice, 50ml methanol three times, 50ml acetone twice (remove residual ...

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Abstract

The invention relates to a preparation method of a molecularly imprinted polymer microsphere in the technical field of the chemical engineering. The invention includes the following steps: under the effect of ultrasound, the mixture is added in the solution and quickly stirred to react for 24 hours; after stirring, filtering and washing, the template molecules are removed by the soxhlet extraction; the polymer removed template molecules are dried to constant weight in vacuum, and the molecularly imprinted polymer microsphere is obtained. The method of separating enrofloxacin from the molecularly imprinted polymer microsphere includes the steps that the molecularly imprinted polymer microsphere of enrofloxacin is filled into the polypropylene solid phase extraction cartridge; the solid phase extraction cartridge is activated and decontaminated, and finally, the enrofloxacin for detecting is eluted and collected. With simple method and perfect mechanical intensity and chemical stability,the invention can be used for the extreme conditions such as acid, alkali, high temperature, etc., and is also applicable to separate, purify and enrich the enrofloxacin in such complex substrates aswater-solubility medium and animal-originated food, thereby possessing a perfect application prospect.

Description

technical field [0001] The invention relates to a preparation method in the technical field of chemical engineering, in particular to a preparation method of molecularly imprinted polymer microspheres and a method for separating enrofloxacin. Background technique [0002] Enrofloxacin (ENR) is a chemically synthesized bacteriostatic agent belonging to the third generation of fluoroquinolones (Fluoroquinolones) antibiotics. It inhibits the synthesis of bacterial DNA by inhibiting bacterial DNA gyrase. It has a strong bactericidal effect and is widely used. It is used in veterinary clinics, but its half-life in animals is relatively long; long-term consumption of human will cause accumulation poisoning. According to the epidemiological survey of this type of drug, its main toxic and side effects include damage to the digestive system, nervous system, liver and kidney function, cardiovascular system, blood system and articular cartilage, and allergic reactions. The allergic re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/26C08F20/06C08F20/14C08F26/06C08F4/04C08F2/44C07D215/56G01N31/00
Inventor 张大兵武爱波瞿国润
Owner SHANGHAI JIAO TONG UNIV
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