丙基乙二胺的QuEChERS凈化管進行基質凈化。采用DB-5MS毛細管色譜柱( 30m×0.25mm , 0.25μm )實現(xiàn)化合物分離,質譜檢測使用多反應監(jiān)測模式,并運用基質匹配標準品校正基質效應。結果:30種農(nóng)藥殘留在0~200ngmL<sup>-1</sup> 時,表現(xiàn)出良好的線性關系,方法的檢出限、定量限及相關系數(shù) (R<sup>2</sup> )均滿足實驗需求。在0.2、0.5mg?kg<sup>-1</sup> 和 1.0mg?kg<sup>-1</sup> 這3個添加水平下,平均回收率為 74.6%~116.0% ,相對標準偏差為 1.1%~ 5.6% 。結論:本方法通過QuEChERS前處理與氣相色譜串聯(lián)質譜聯(lián)用技術,實現(xiàn)了香辛料基質中多類別農(nóng)藥殘留的高通量檢測,其靈敏度滿足我國《食品安全國家標準 食品中農(nóng)藥最大殘留限量》(GB 2763—2021)最大殘留限量要求,可為食品監(jiān)管機構提供可靠的技術支持。-龍源期刊網(wǎng)" />

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QuEChERS結合氣相色譜串聯(lián)質譜 測定香辛料中30種農(nóng)藥殘留

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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

香辛料作為食品風味調控的核心要素,不僅賦予菜肴獨特的揮發(fā)性風味特征,其含有的生物活性成分(如辣椒素、姜酚等)更被證實具有促消化、抗氧化等生理功能[1-3]。(剩余4975字)

目錄
monitor