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Preparation method and application of molecularly imprinted polymer of penicillin antibiotics and intermediate of penicillin antibiotics

A technology of imprinting polymers and molecular imprinting, applied in chemical instruments and methods, other chemical processes, etc., to achieve the effect of good identification performance

Inactive Publication Date: 2013-02-13
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology has been applied to the preparation of solid-phase extraction columns for a single target compound, but there is no report on the preparation of molecularly imprinted solid-phase extraction columns for the separation of multiple compounds and their intermediates at the same time

Method used

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  • Preparation method and application of molecularly imprinted polymer of penicillin antibiotics and intermediate of penicillin antibiotics
  • Preparation method and application of molecularly imprinted polymer of penicillin antibiotics and intermediate of penicillin antibiotics
  • Preparation method and application of molecularly imprinted polymer of penicillin antibiotics and intermediate of penicillin antibiotics

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 5 mL of methanol, formic acid, ethanol, dichloromethane, N,N-dimethylamide, methanol / water (7 / 3), acetonitrile, acetonitrile / water (7 / 3), acetonitrile / Water (8 / 2) was used as the solvent to investigate the dissolving effects of different solvents on 6-APA and MAA, see Table 1. Because the template molecule 6-APA is not completely soluble in organic solvents, and slightly soluble in water, it decomposes with alkali and is relatively stable to acids, so formic acid was selected as the porogen.

[0022] Table 1 Dissolving effect of different solvents on 6-APA and MAA

[0023]

[0024] (2) The effect of the ratio of the amount of functional monomer MAA to the template molecule 6-APA: the experiment fixed the amount of the template molecule, changed the amount of the functional monomer, and investigated the molar ratio of the functional monomer to the template molecule as 3:1, 5:1 , 7:1, and 9:1, the interaction between the functional monomer and the template mo...

Embodiment 2

[0038] The packing effects of MIPs and diatomaceous earth with mass ratios of 1:1, 2:3, 2:1, and 3:1 were compared. The rate of the sample solution passing through the molecularly imprinted solid phase extraction column (MISPE) and the adsorption effect on the template molecules were compared, and the results are shown in Table 3.

[0039]Table 3 Selection of Preparation Conditions for Molecularly Imprinted Polymer SPE Columns

[0040] Polymer: diatomaceous earth 1：1 3：2 2：1 3：1 Filtration rate (mL / min) 2 1.6 1 0.3 Adsorption capacity (umol / g) 15.6 19.2 24.5 25.0

[0041] It can be seen from Table 3 that when the ratio of MIPs to diatomaceous earth is 3:1, the adsorption effect of MISPE is better, but the sample loading rate is too slow. When the ratio is 1:1 and 3:2, although the sample passing rate Faster but less effective. Therefore, the optimal ratio is chosen to be 2:1.

[0042] Preparation of 6-APA molecularly imprinted solid-phase...

Embodiment 3

[0044] (1) Accurately weigh 0.22 g of the template molecule 6-aminopenicillanic acid (6-APA) and dissolve it in a container containing 10 mL of formic acid, add 0.44 mL of functional monomer methacrylic acid (MAA), and incubate at room temperature Vibrate in an ultrasonic instrument for 30 minutes to fully combine the template molecules with the functional monomers; then add 3.86 mL of cross-linking agent ethylene glycol dimethacrylate (EDMA) and 0.05 g of azobisisobutyronitrile (AIBN) into the container , mix evenly, ultrasonically oscillate for 15 min, and fill the container with N 2 And sealed, heated in a 60 °C water bath for 24 h to obtain a white solid polymer;

[0045] (2) Crush the white solid polymer obtained in step (1), grind it through a 220 mesh (particle size 0.065 mm) sieve, use acetonitrile-water or volume ratio of 8:2 or 7:3 or 6:3 The template molecule 6-APA in the polymer was eluted with a 6:4 methanol / acetic acid solution, and then the solvent was eluted w...

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Abstract

The invention relates to a preparation method of molecularly imprinted polymer of penicillin antibiotics and intermediate of penicillin antibiotics. The molecularly imprinted polymer is prepared from 6-aminopenicilanic acid (6-APA) as template molecule, methacrylic acid (MAA) as functional monomer and ethylene glycol dimethacrylate as cross-linking agent by dissolving, polymerization, elution, and the like. The molecularly imprinted polymer is used as filler of solid phase extraction (SPE) column, and the prepared solid phase extraction column has good recognition on penicillin antibiotics, such as penicillin-G potassium (PEN), ampicillin (AMP), amoxicillin (AMO) and intermediate 6-APA of penicillin antibiotics, and can be used for sample pretreatment in detection of penicillin antibiotics residue in animal-derived food.

Description

technical field [0001] The invention relates to a preparation method of a molecularly imprinted polymer; specifically, a method for preparing a molecularly imprinted polymer of a penicillin antibiotic and its intermediate in animal-derived food. Background technique [0002] Penicillin antibiotics are a class of broad-spectrum antibiotics containing the core structure of 6-aminopenicillanic acid (6-APA), and have strong antibacterial effects on both Gram-positive and Gram-negative bacteria, so they are widely used in veterinary clinic. Improper use of penicillin antibiotics in animal feeding will lead to food safety issues of animal origin. [0003] Molecular Imprinting Technology (MIT) is a new technology for the preparation of polymer materials with recognition function that has emerged in recent years. It can obtain molecularly imprinted polymers (molecularly imprinted polymers, MIPs). This technology has been applied to the preparation of solid-phase extraction column...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F222/14C08J9/26B01J20/285B01J20/30
Inventor 檀华蓉司雄元田春秋苏红晓祁克宗
Owner ANHUI AGRICULTURAL UNIVERSITY
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