Efficient separation and purification method for multi-residue sulfonamide antibiotics in biological samples

A technology for separation and purification of biological samples, applied in the field of enrichment and purification, rapid separation, and high selectivity of sulfonamide antibiotic residues. good enrichment effect

Inactive Publication Date: 2011-12-14
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecularly imprinted polymer in this application is only capable of recognizing sulfamethoxazole, but not other sulfonamide antibiotics

Method used

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  • Efficient separation and purification method for multi-residue sulfonamide antibiotics in biological samples
  • Efficient separation and purification method for multi-residue sulfonamide antibiotics in biological samples
  • Efficient separation and purification method for multi-residue sulfonamide antibiotics in biological samples

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Experimental program
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preparation example Construction

[0020] The preparation methods of molecularly imprinted polymers in the following examples are as follows:

[0021] Weigh an appropriate amount of functional monomer methacrylic acid and template molecule sulfadimethoxine (SDM) and dissolve them in 15 mL of acetonitrile diluent, add 5 mL of cross-linking agent ethylene glycol dimethacrylate EGDMA, azobisisobutyronitrile to initiate Dose 120mg, ultrasonic degassing for 5-10 minutes, after mixing evenly, pass nitrogen gas for 10-15 minutes, and seal. Put it in a water bath at 60°C for 24 hours; after the polymerization reaction, take out the synthesized block polymer, grind it, sieve it, and use methanol: formic acid (90:10, v / v) and methanol to remove the template molecule through Soxhlet extraction. , repeated sedimentation with acetone to remove superfine polymer particles, and then vacuum-dry the polymer without template molecules at 50°C to obtain a molecularly imprinted polymer with specific recognition function for sulfon...

Embodiment 1

[0023] (1) Preparation of molecularly imprinted polymers for sulfonamide antibiotics

[0024] Accurately weigh 2mmol of functional monomer methacrylic acid and 1mmol of template molecule sulfadimethoxine and dissolve in 15mL of acetonitrile, add 25mmol of cross-linking agent EGDMA, 120mg of initiator azobisisobutyronitrile, ultrasonically degas for 5min, and mix well , into the nitrogen 10 ~ 15min, sealed. Put it in a water bath at 60°C for 24 hours; after the polymerization reaction, take out the synthesized block polymer, grind it, sieve it, and use methanol: formic acid (90:10, v / v) and methanol to remove the template molecule through Soxhlet extraction. , repeated sedimentation with acetone to remove superfine polymer particles, and then vacuum-dried the polymer from which template molecules were removed at 50° C. to obtain molecularly imprinted polymers.

[0025] (2) sulfa antibiotic matrix solid-phase dispersion extraction method, concrete steps are as follows

[0026]...

Embodiment 2

[0033] (1) Preparation of molecularly imprinted polymers for sulfonamide antibiotics

[0034] Accurately weigh 4mmol of functional monomer methacrylic acid and 1mmol of template molecule sulfadimethoxine and dissolve in 15mL of acetonitrile, add 25mmol of crosslinking agent EGDMA, 120mg of initiator azobisisobutyronitrile, ultrasonically degas for 5-10min, mix After uniformity, nitrogen gas was introduced for 15 minutes and sealed. Put it in a water bath at 60°C for 24 hours; after the polymerization reaction, take out the synthesized block polymer, grind it, sieve it, and use methanol: formic acid (90:10, v / v) and methanol to remove the template molecule through Soxhlet extraction. , repeated sedimentation with acetone to remove superfine polymer particles, and then vacuum-dried the polymer from which template molecules were removed at 50° C. to obtain molecularly imprinted polymers.

[0035] (2) sulfa antibiotic matrix solid-phase dispersion extraction method, concrete step...

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PUM

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Abstract

The invention relates to a method for efficiently separating and purifying multiresidue sulfonamide antibiotics in a biological sample. The method is characterized by comprising the following steps of: (1) preparing a molecular imprinted polymer, comprising the steps of burdening according to the mol ratio of template molecule to functional monomer to cross linking agent of being 1: (2-8): 25 and obtaining the molecular imprinted polymer with special identification function to the sulfonamide antibiotics by adopting a body polymerization method; (2) weighing certain amount of biological sample to be separated into a mortar, grinding the biological sample by the mortar, adding right amount of the molecular imprinted polymer, and further homogenating to obtain a homogenated sample, wherein the weight ratio of the biological sample to be separated to the molecular imprinted polymer is 2: (1-5), and (3) placing the homogenated sample in a solid phase extraction column, sequentially rinsing with 2.0-4.0ml of water, 2.0-4.0ml of 10wt% acetonitrile aqueous solution, and then eluting with 3.0-5.0ml of methanol/methanoic acid mixed solution; and separating the sulfonamide antibiotics from the biological sample to be separated by being instantly dissolved in the methanol/methanoic acid mixed solution. The method provided by the invention has wide selectivity and good separation and purification effect.

Description

technical field [0001] The invention relates to the fields of analytical chemistry, food safety and veterinary drug residues, in particular to a highly selective, rapid separation, enrichment and purification method for multiple residues of sulfonamide antibiotics in complex biological samples. Background technique [0002] Sulfonamides (SAs) are a class of chemically synthesized antibiotics, which have inhibitory effects on most Gram-positive bacteria and some Gram-negative bacteria, and are widely used in the treatment of bacterial infections in various animals. However, sulfonamide antibiotics can cause allergic reactions in the body, damage the hematopoietic system of the body, and lead to the occurrence of various anemias. In particular, the problem of antibiotic residues in food is very common at present. Many countries in the world have made strict regulations on the antibiotic residue limits in animal-derived foods. Canada, the European Union, the United States and o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/14B01J20/285B01J20/30
Inventor 孟原史西志孙爱丽李德详陈炯
Owner NINGBO UNIV
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