Method for detecting neonicotinoid insecticides and metabolites in urine by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry

An ultra-high-efficiency liquid phase and neonicotinoid technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of easily damaged chromatographic columns, mass spectrometers, and poor stability of instruments, and achieve accurate and reliable detection results. Improved matrix effect and good linearity

Pending Publication Date: 2021-06-22
CHONGQING MEDICAL UNIVERSITY
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Problems solved by technology

If it is used for urine testing of a large sample population, it is easy to damage the chromatographic column and mass spectrometer, resulting in a gradual deterioration of the stability of the instrument

Method used

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  • Method for detecting neonicotinoid insecticides and metabolites in urine by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting neonicotinoid insecticides and metabolites in urine by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting neonicotinoid insecticides and metabolites in urine by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry

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Embodiment 1

[0038] 1 Experimental instruments and equipment

[0039] The experimental instruments and equipment used in the present invention are shown in Table 1.

[0040] Table 1 Experimental instruments and equipment

[0041]

[0042] 2 Experimental reagents and materials

[0043] The experimental reagents and materials used in the present invention are shown in Table 2.

[0044] Table 2 Experimental reagents and materials

[0045]

[0046]

[0047] The source of the urine sample to be tested is: the urine sample of a middle school student volunteer in Chongqing.

[0048] 3 Preparation of standard solutions and reagents used

[0049]Weigh 10 standard neonicotinoid insecticides (imidacloprid, acetamiprid, thiamethoxam, nitenpyram, thiacloprid, clothianidin, dinotefuran) with an electronic analytical balance (1 / 10,000). , chlorothialine, flonicamid, sulfonicaflor), 2 metabolites (2-imidazolidinone, demethyl acetamiprid), 1 isotope internal standard (acetamiprid-d 3 ), were...

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Abstract

The invention discloses a method for detecting neonicotinoid insecticides and metabolites in urine by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry. The method comprises the following steps: (1) preparing an internal standard stock solution and a target analyte standard stock solution; (2) pretreating a urine sample to be detected: 1) performing enzymolysis; 2) performing solid-phase extraction, separation and purification: a) activating a solid-phase extraction small column; b) loading a sample; c) performing elution: eluting the substance to be detected by using a dichloromethane-acetonitrile mixture, wherein the volume ratio of dichloromethane to acetonitrile is (8-5):(2-5); 3) extracting, crystallizing and removing impurities: blow-drying eluent, adding the dichloromethane-acetonitrile mixture to dissolve residues, centrifuging, taking supernate, blow-drying, and re-dissolving with methanol-formic acid water to obtain re-dissolved liquid, and obtaining the methanol-formic acid water by mixing methanol and a formic acid water solution with the concentration of 0.15% according to the volume ratio of (1-2):(9-8); 4) filtering with a filter membrane; (3) analyzing a urine sample; (4) drawing a standard curve; and (5) performing data analysis.

Description

technical field [0001] The invention relates to the technical field of pesticide detection, in particular to a method for detecting neonicotinoid pesticides and metabolites in urine by solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Neonicotinoid insecticides are a new class of insecticides developed and put into use at the end of the 20th century. This type of insecticide has a novel and unique mode of action, high efficiency and rapid insecticidal efficiency, and is not easy to produce cross-resistance with traditional pesticides. Once it comes out, it has become the fastest growing and largest class of insecticides in the market. [0003] However, after three decades of frequent use, its toxic effects on non-target organisms and the human body have gradually attracted social attention. A large number of in vivo and in vitro experiments have revealed that neonicotinoid insecticides have potential ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 高洁莹周文莉郑美琳岳敏贾燕
Owner CHONGQING MEDICAL UNIVERSITY
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