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Preparation method and application for aminoglycoside-antibiotic molecularly imprinted polymers

A technology of aminoglycosides and molecular imprinting, which is applied in the field of analytical chemistry, can solve problems such as the preparation method of molecularly imprinted polymers that have not yet been seen in aminoglycoside antibiotics, and achieve the effect of high extraction recovery

Inactive Publication Date: 2013-07-31
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no reports on the preparation of molecularly imprinted polymers of aminoglycoside antibiotics and their use as solid-phase extraction materials

Method used

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  • Preparation method and application for aminoglycoside-antibiotic molecularly imprinted polymers
  • Preparation method and application for aminoglycoside-antibiotic molecularly imprinted polymers
  • Preparation method and application for aminoglycoside-antibiotic molecularly imprinted polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1. Preparation method of aminoglycoside antibiotic molecularly imprinted polymer

[0021] (1) Dissolve 1-5mmol of streptomycin template molecules in 10mL of pure water, add 4-20mmol of functional monomer methacrylic acid, and stir the mixed solution at room temperature for 30min, so that the template molecules and functional monomers are fully Mix; then add 15-90ml of cross-linking agent ethylene glycol dimethacrylate and 20-100mL of methanol solvent; then add 5mmol of azobisisonitrile, and ultrasonically shake the resulting solution for 10min to make it evenly mixed, blow with nitrogen for 15min; The reaction solution was placed in a water bath at 60°C and stirred and heated at 1000 rpm for 24 hours to obtain a white solid polymer;

[0022] (2) After crushing and grinding the white solid polymer obtained in step (1) through a 75-mesh sieve, add it to a round-bottomed flask filled with 4M hydrochloric acid-methanol with a volume ratio of 1:1 and heat it under re...

Embodiment 2

[0024] Example 2. MIP verification of the extraction effect of aminoglycoside antibiotics

[0025] (1) After measuring the adsorption properties of molecularly imprinted polymers on template molecules at different ratios, the optimal ratio of template molecules: functional monomers: crosslinking agents = 1:14:60 was finally established. The resulting molecularly imprinted polymers (MIPs) were characterized by infrared spectroscopy, see figure 1 . It can be seen from the infrared spectrum that the materials before and after the eluted template molecules contain a wavenumber of 1638.63cm -1 It is a carbon-carbon double bond peak, and a wavenumber of 3441.76cm is added to the infrared spectrum of MIP after template removal -1 The peak, by 3441.76cm -1 、1732.5cm -1 、1259.65cm -1 These three peaks can confirm that carboxyl groups have been added in the eluted material structure, indicating that the template molecules in the obtained MIP material have been completely removed. ...

Embodiment 3

[0029] Example 3. MIP column detects commercially available honey

[0030] (1) Fill 200 mg of the molecularly imprinted polymer (MIP) obtained above into a 3 mL small column empty tube as a solid phase extraction (SPE) column filler to make an SPE small column. Activate with 3mL methanol and 3mL water first; then use a concentration of 20mmol / L K 2 HPO 4 The buffer solution (pH=7.4) was loaded, rinsed with 3mL water, and finally eluted with a mixture of FA / ACN=20 / 80 (v / v). The eluate was analyzed and detected by LC-MS / MS.

[0031] (2) Prepare standard solution: Prepare 4 μg / mL mixed standard solution with 0.1 mg / mL four aminoglycoside mycin stock solutions, and then prepare a series of standard concentration solutions step by step.

[0032] (3) Accurately weigh 2g of the blank honey sample, place it in a 15mL polypropylene plastic tube, and then add 5mL of it to a concentration of 20mmol K 2 HPO 4 The buffer solution was vortexed for 30 s, and then centrifuged at 4500 rpm...

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Abstract

The invention discloses a preparation method and application for aminoglycoside-antibiotic molecularly imprinted polymers. The target molecularly imprinted polymers with the fixed hole sizes and the fixed shapes are made with streptomycin as template molecules, methacrylic acid as functional monomers and ethylene glycol dimethacrylate as cross-linking agents in a thermal initiation polymerization mode, and are used as solid phase extraction column packing. High-selectivity enrichment of aminoglycoside antibiotics can be conducted by a produced solid phase extraction column. The aminoglycoside-antibiotic molecularly imprinted polymers are high in antibiotic extraction recovery rate, and can be used for sample pretreatment of detection of aminoglycoside antibiotics in animal derived food.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a preparation method and application of molecularly imprinted polymers for determining aminoglycoside antibiotics in animal source foods. Background technique [0002] Molecularly imprinted polymers (molecularly imprinted polymers, MIP) is a new type of polymer material that can be obtained in spatial structure and binding sites that completely matches specific molecules and has highly selective recognition functions. The high selectivity of MIP can be used as solid phase extraction to selectively adsorb target sample molecules from complex sample matrices, and is very suitable for complex sample pretreatment and enrichment. [0003] As a broad-spectrum antibiotic, aminoglycoside antibiotics are very common in foods represented by meat products. Due to the complex structure of aminoglycoside antibiotics and the extremely complex food matrix itself, traditional solid-phase ext...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/26B01J20/26B01J20/30
Inventor 章飞芳纪顺利朱英鹏张诗芸郭碧泽杨丙成梁鑫淼
Owner EAST CHINA UNIV OF SCI & TECH
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