QuEChERS结合气相色谱串联质谱 测定香辛料中30种农药残留

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Determination of 30 Pesticide Residues in Spices by QuEChERS Combined with Gas Chromatography-Tandem Mass Spectrometry
ZHANG Jie, YAN Jun, ZHAO Bo,PENG Tao, WANG Xingzhi*
(Lanzhou Institute ofFood and Drug Inspection and Testing, Key Laboratory of Pesticide and Veterinary Drug
Monitoring, State Administration for Market Regulation, Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines,Lanzhou 73oo50, China)
Abstract: Objective: To establish a gas chromatography-tandem mass spectrometry method for the determination of 30 common pesticide residues in spices. Method: Samples were hydrated for 30min , extracted with 1% acetic acid-acetonitrile via vortex-assisted extraction, and purified using a QuEChERS cleanup tube containing 150mg anhydrous magnesium sulfate and 50mg primary secondary amine. Compound separation was achieved usinga DB-5MS capillary column (30m×0.25mm , 0.25μm ,andmass spectrometry detection wasperformed in multiple reaction monitoring mode with matrix-matched calibration standards to corrct for matrix efects. Result: The 30 pesticides exhibited good linearity within the concentration range of 0~200ng⋅mL-1 . The method's limits of detection, limits of quantification, and correlation coefficients (R2) all met experimental requirements.At spiked levels of 0.2, 0.5mg⋅kg-1 and 1.0mg⋅kg-1 ,the average recoveries ranged from 74.6% to 116.0% ,with relative standard deviations of 1.1% to 5.6% . Conclusion: This method combines QuEChERS pretreatment with gas chromatographytandem mass spectrometry to achieve high-throughput detection of multiclasspesticide residues in spice matrices.
Its sensitivity complies with the maximumresidue limits specifed inGB2763—2021,providing reliable technical support for food regulatory agencies.
Keywords: spices; pesticide residues; gas chromatography-tandem mass spectrometry; QuEChERS
香辛料作为食品风味调控的核心要素,不仅赋予菜肴独特的挥发性风味特征,其含有的生物活性成分(如辣椒素、姜酚等)更被证实具有促消化、抗氧化等生理功能[1-3]。(剩余4975字)