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Method for detecting residual quantities of sulfonamides, quinolones and tetracyclines in vegetables

A technology of quinolones and tetracyclines, which is applied in the field of detection of sulfonamides, quinolones and tetracyclines residues in vegetables, can solve the problems of single type of antibiotics, poor separation and extraction effect of pretreatment, etc., to eliminate matrix influence and reduce interference , good separation effect

Pending Publication Date: 2021-03-26
秦皇岛市农产品质量安全监督检验中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a method for detecting residual amounts of sulfonamides, quinolones and tetracyclines in vegetables, which solves the problems of poor pretreatment separation and extraction effects and single detection of antibiotics in the prior art

Method used

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  • Method for detecting residual quantities of sulfonamides, quinolones and tetracyclines in vegetables
  • Method for detecting residual quantities of sulfonamides, quinolones and tetracyclines in vegetables
  • Method for detecting residual quantities of sulfonamides, quinolones and tetracyclines in vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Pass the mixed standard solution with a concentration of 10ug / L through a 0.22 μm syringe filter into a brown sample bottle, and then use high performance liquid chromatography-tandem mass spectrometry to simultaneously determine the content of 34 antibiotics in the mixed standard solution. The specific conditions are as follows:

[0057] ① Chromatographic conditions:

[0058] Chromatographic column: Phenomenex Kinetex F5 (3.0×50mm, 2.6μm);

[0059] Mobile phase: A: 0.1% formic acid aqueous solution, B: acetonitrile;

[0060] Gradient elution program: 0~0.25min, 10%B; 0.25~6min, 10%~30%B; 6~9min, 30%~50%B; 9~10min, 50%~90%B; 10~11min , 90% B; 11.01-13min, 10% B;

[0061]Flow rate: 0.3mL / min; Column temperature: 30℃; Injection volume: 5μL

[0062] ②Mass spectrometry conditions:

[0063] Electrospray ionization source (ESI), positive ion mode;

[0064] Ion source temperature: 550°C;

[0065] Spray voltage: 5500V;

[0066] Air curtain air pressure is 206.8kPa;

[0...

Embodiment 2

[0071] The chromatographic column in Example 1 was replaced by ACQUITY UPLC BEH C18 (2.1×100mm, 1.7 μm), and the others remained the same as in Example 1.

[0072] The results show that the ACQUITY UPLC BEH C18 column has a good separation effect on most of its compounds, but it is difficult to achieve the separation of sulfamethoxine and sulfamethoxypyridazine. Quantitative analysis of the influence between. However, the Phenomenex Kinetex F5 chromatographic column can better separate these two isomers, because the pentafluorophenyl stationary phase used in the Phenomenex Kinetex F5 chromatographic column is suitable for halogenated compounds, conjugated compounds, isomers or strong poles. The analysis of neutral compounds, especially the isomers of different positions of the substituents of the benzene ring, can achieve better separation effect. Therefore, the present invention has finally selected the Phenomenex Kinetex F5 (3.0 × 50mm, 2.6 μm) chromatographic column to sep...

Embodiment 3

[0074] The mobile phase B of Example 1 was replaced by methanol, and other operations were the same as in Example 1.

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Abstract

The invention relates to the technical field of antibiotic detection, and provides a method for detecting residual quantities of sulfonamides, quinolones and tetracyclines in vegetables; the method comprises the following steps: S1, performing sample pretreatment: taking a vegetable sample, performing freeze-drying, performing grinding, and performing screening to obtain a screened sample; S2, performing crude extraction of the sample: adding an extracting agent into the screened sample to extract the sample; S3, carrying out secondary extraction; S4, performing concentrating, fixing the volume and performing filtering; and S5, carrying out high performance liquid chromatography-tandem mass spectrometry analysis to obtain the residual quantity. By means of the technical scheme, the problems that in the prior art, a pretreatment means is complex, good separation and extraction cannot be achieved, and the variety of detected antibiotics is single are solved.

Description

technical field [0001] The invention relates to the technical field of antibiotic detection, in particular to a method for detecting residues of sulfonamides, quinolones and tetracyclines in vegetables. Background technique [0002] Antibiotics refer to secondary metabolites produced by microorganisms or higher animals and plants in the course of life, or analogs synthesized artificially based on the chemical structure of antibiotics. Antibiotics can continue to accumulate along with the transmission of the food chain, and when they reach a certain concentration, they will seriously endanger human health. With the continuous improvement of people's living standards, people pay more and more attention to balanced nutrition, and the demand for vegetarian vegetables is gradually increasing. At the same time, food safety issues caused by antibiotics are also increasingly concerned by everyone. Therefore, it is necessary to continuously optimize the analysis and detection techno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李曼张嘉楠曹秀梅李宏娟杨赵伟张珍珍王爱卿段培姿马珊珊王狄李博侯桂双陈军王艳华郭万加
Owner 秦皇岛市农产品质量安全监督检验中心
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