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Method for non-targeted quick screening of unknown residual pesticides in imported grains by FaPEx-UPLC-Q-TOF

A pesticide residue, non-targeted technology, applied in the field of pesticide detection, can solve the problems of complex matrix, interference with target analysis, chromatographic column and mass spectrometry damage, etc., to achieve good stability, improve accuracy, and avoid false positive results.

Active Publication Date: 2017-06-27
舟山出入境检验检疫局综合技术服务中心
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Problems solved by technology

[0004] However, the matrix of grain samples is complex and contains substances such as protein and fat, which will not only interfere with the analysis of the target (pesticide compound), but also cause fatal damage to the chromatographic column and mass spectrometer. Therefore, how to effectively extract the target and purify and remove the Interfering impurities have become a problem that needs to be solved urgently

Method used

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  • Method for non-targeted quick screening of unknown residual pesticides in imported grains by FaPEx-UPLC-Q-TOF
  • Method for non-targeted quick screening of unknown residual pesticides in imported grains by FaPEx-UPLC-Q-TOF
  • Method for non-targeted quick screening of unknown residual pesticides in imported grains by FaPEx-UPLC-Q-TOF

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Experimental program
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Embodiment

[0034] 1.1 Reagents and medicines

[0035]Pesticide standard substance (purity ≥ 95%, Dr. Ehrenstorfer company). The single-standard stock solution (1000mg / L) was prepared from methanol, acetonitrile or acetone, and all standard solutions were stored at 4°C in the dark. Acetonitrile (chromatographically pure, Fisher, USA); ultrapure water (Millipore system); acetic acid (AR). FaPEx (Fast Pesticide Extraction kits) cartridge (30mg, 6mL, Giant Research Technology Co., Ltd.)

[0036] 1.2 Imported grain samples are sorghum, barley, wheat, soybean, corn, and rapeseed. The importing countries are the United States, France, Australia, Canada, Ukraine, Brazil, Argentina, and Uruguay. They are collected at my country's grain import ports.

[0037] 1.3 Instruments and equipment Agilent 6550ifunnel / QTOF liquid chromatography-quadrupole time-of-flight mass spectrometer, equipped with dual jet stream electrospray ionization (Dual AJS ESI) source (Agilem, USA).

[0038] 1.4 Sample pretre...

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Abstract

The invention relates to the field of pesticide detection and discloses a method for non-targeted quick screening of unknown residual pesticides in imported grains by FaPEx-UPLC-Q-TOF. The method for the non-targeted quick screening of the unknown residual pesticides in the imported grains is established by using a FaPEx-UPLC-Q-TOF principle. The method comprises the following steps: extracting the unknown residual pesticides in the imported grains by adopting an acetic acid and acetonitrile solution; carrying out purification and concentration by using a FaPEx solid-phase extraction column; detecting by UPLC-Q-TOF; carrying out database matching by using an exact mass number of characteristic ions of a target compound, isotope matching, secondary fragment information and retention time, and screening suspected unknown pesticides. The result shows that by using the method, the residual pesticides in the imported grains can be quickly screened without a reference standard substance. The method has the advantages of quickness, accuracy and high analysis throughput, and can provide an important method and basis for quick screening and quality control of the residual pesticides in the imported grains.

Description

technical field [0001] The invention relates to the field of pesticide detection, in particular to a FaPEx-UPLC-Q-TOF non-targeted rapid screening method for unknown pesticide residues in imported grains. Background technique [0002] Under the situation of international trade integration, the import of grain and cereal products has increased rapidly. In 2015, imported grain has exceeded 120 million tons, becoming the largest category of imported food and agricultural products, which reflects the rigid demand for domestic grain. At the same time, people pay more and more attention to food quality and safety, and public opinion also attaches great importance to the safety of imported food, and pesticide residues are one of the important factors affecting the quality and safety of imported food. From 2010 to 2014, the detection rate of various pesticide residues (deltamethrin and fenitrothion) was as high as 8.6% in grains imported through Qingdao, Shenzhen and Qinhuangdao por...

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Application Information

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IPC IPC(8): G01N30/06G01N30/89
CPCG01N30/06G01N30/89G01N2030/062
Inventor 周秀锦陈宇杨赛军邵宏宏张静其他发明人请求不公开姓名
Owner 舟山出入境检验检疫局综合技术服务中心
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