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Efficient method for extracting sulfonamide residues in animal derived food

A sulfonamide drug and animal-derived technology, applied in solvent extraction, separation methods, chemical instruments and methods, etc., can solve the problems of sample liquid emulsification, loss of sample information, complicated operation steps, etc., and achieve mild reaction and high polymer yield High and stable effect

Active Publication Date: 2016-07-20
CHINA PHARM UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the solid-phase extraction material (MCX) stipulated by the existing national standard method has complicated operation steps when enriching the sulfonamide drug residues in the lipid-rich matrix, and still needs to degrease through n-hexane. This step often causes the sample liquid to emulsify and lose part Sample information

Method used

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  • Efficient method for extracting sulfonamide residues in animal derived food
  • Efficient method for extracting sulfonamide residues in animal derived food
  • Efficient method for extracting sulfonamide residues in animal derived food

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1 (13 kinds of sulfonamide drug residue analysis in the pork sample)

[0033] 1) Synthesis of sulfonic acid polystyrene polymer: 5.0mL styrene monomer, 1.0g sodium 4-vinylbenzenesulfonate and 0.30g sodium carbonate were placed in a triangular reaction flask, and 20mL ultrapure water was added , and reacted at 65°C with magnetic stirring for 10 minutes, then added 0.20 g of ammonium persulfate initiator, and continued to react at 65°C with magnetic stirring for 12 hours. Stop stirring after the reaction is over, cool the milky white suspension to room temperature, add 2mL formic acid to break the emulsion, mix well and let it stand for a while, centrifuge (16000r / min, 30min), discard the supernatant, take the lower layer and put it in The beaker is washed with water and placed in a vacuum drying oven to dry at 55°C, ground into powder, and then the above washing-drying-grinding steps are repeated twice to obtain the final product.

[0034] 2) Preparation of p...

Embodiment 2

[0052] Embodiment 2 (13 kinds of sulfonamide drug residue analysis in the chicken sample)

[0053] 1) Synthesis of sulfonic acid-based polystyrene polymer: 2.5mL styrene monomer, 0.5g sodium 4-vinylbenzenesulfonate and 0.15g sodium carbonate were placed in a triangular reaction flask, and 10mL ultrapure water was added , and reacted at 75°C with magnetic stirring for 10 minutes, then added 0.20 g of sodium persulfate initiator, and continued to react at 75°C with magnetic stirring for 24 hours. Stop stirring after the reaction is over, cool the milky white suspension to room temperature, add 1mL acetic acid to break the emulsion, mix well and let it stand for a while, centrifuge (14000r / min, 30min), discard the supernatant, take the lower layer and put it in The beaker is washed with water and placed in a vacuum drying oven to dry at 60°C, ground into powder, and then the above washing-drying-grinding steps are repeated twice to obtain the final product.

[0054]2) Preparatio...

Embodiment 3

[0060] Embodiment 3 (13 kinds of sulfonamide drug residue analysis in the beef sample)

[0061] 1) Synthesis of sulfonic acid polystyrene polymer: 5.0mL styrene monomer, 1.0g sodium 4-vinylbenzenesulfonate and 0.30g sodium carbonate were placed in a triangular reaction flask, and 20mL ultrapure water was added , and reacted at 65°C with magnetic stirring for 10 minutes, then added 0.20 g of ammonium persulfate initiator, and continued to react at 65°C with magnetic stirring for 12 hours. Stop stirring after the reaction is over, cool the milky white suspension to room temperature, add 2mL formic acid to break the emulsion, mix well and let it sit for a while, centrifuge (18000r / min, 30min), discard the supernatant, take the lower layer and put it in The beaker is washed with water and placed in a vacuum drying oven to dry at 55°C, ground into powder, and then the above washing-drying-grinding steps are repeated twice to obtain the final product.

[0062] 2) Preparation of pol...

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Abstract

The invention belongs to the technical field of sample pretreatment in analytical chemistry, and relates to an efficient method for extracting sulfonamide residues in animal derived food. The efficient method includes synthesizing a sulfonic polystyrene high-molecular polymer, preparing a nanofiber membrane from the sulfonic polystyrene high-molecular polymer through electrostatic spinning, and treating the surface of the nanofiber membrane with plasmas. The high-hydrophilia and high-stability sulfonic functional group nanofiber membrane is prepared, and a sample pretreatment method for effectively enriching sulfonamide type veterinary drug residues without degreasing steps is created. By the sulfo group modified hydrophilia nanofiber membrane, efficient enrichment, extraction and analysis of the sulfonamide type veterinary drug residues of 13 types of labeled samples and market samples in the animal derived food can be realized. By the method, the sulfonamide residues in fat-rich animal derived food base materials can be enriched selectively, utilization of normal hexane is not needed, operation steps are reduced, emulsification is avoided, and accordingly, extraction efficiency is improved remarkably; the method has the advantages of rapidness, simplicity, convenience, high efficiency and high repeatability.

Description

technical field [0001] The invention provides a sample pretreatment method for efficiently extracting sulfonamide drug residues in animal-derived food based on a sulfonic acid group highly hydrophilic functionalized nanofiber membrane, which belongs to the technical field of sample pretreatment in analytical chemistry. Background technique [0002] Veterinary drugs play a very important role in preventing and controlling animal diseases, increasing production efficiency, and improving the quality of animal products. However, the abuse of veterinary drugs can easily lead to the residue of harmful substances in animal source food, which not only causes direct harm to human health, but also causes great harm to the development of animal husbandry and the ecological environment. With the transformation of people's demand for animal-sourced foods to quality-based ones, veterinary drug residues in animal-sourced foods have gradually become an important focus of food safety issues....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/00B01D15/08G01N30/02G01N30/06
CPCB01D11/00B01D15/08G01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 陈蓉曲斌沈卫阳杨盈盈李悦陆勇刘晓楠
Owner CHINA PHARM UNIV
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