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气相色谱-串联质谱法测定牛奶中氯菊酯及其代谢物残留。

Determination of chlordimeform and its metabolite residue in milk by gas chromatography-tandem mass spectrometry.

机构信息

Key Laboratory of Pollution Exposure and Health Intervention of Zhejiang Province, College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China.

Technical Center of Hangzhou Customs, Hangzhou 310008, China.

出版信息

Food Res Int. 2024 Sep;192:114754. doi: 10.1016/j.foodres.2024.114754. Epub 2024 Jul 16.

Abstract

Herein, the determination of chlordimeform and its metabolite 4-chloro-2-methylaniline residue in milk was performed for the first time using gas chromatography-tandem mass spectrometry (GC-MS/MS). Samples were extracted using acetonitrile, and cleaned using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Separation was performed using the DB-17 MS column. It was detected in a selected reaction monitoring (SRM) mode and quantified using a matrix-matched isotope internal standard method. Under optimal conditions, a good linear relationship was observed in the concentration range of 10-200 µg/kg. The limit of quantitation was 10.0 µg/kg. The spiked recoveries for the target substance ranged from 84.5 % to 107.3 %, with relative standard deviations (RSD) of <7.2 %. The spiked samples were further confirmed by gas chromatography-quadrupole-Orbitrap high-resolution mass spectrometry (GC-Orbitrap HRMS). The combined method resulted in high accuracy and sensitivity and was suitable for the determination of chlordimeform and its metabolite 4-chloro-2-methylaniline residue in milk.

摘要

本文首次采用气相色谱-串联质谱法(GC-MS/MS)测定牛奶中林丹和其代谢物 4-氯-2-甲基苯胺残留量。样品用乙腈提取,采用快速、简单、廉价、有效、耐用和安全(QuEChERS)方法净化。采用 DB-17 MS 柱进行分离,在选择反应监测(SRM)模式下进行检测,并采用基质匹配同位素内标法进行定量。在最佳条件下,浓度范围在 10-200μg/kg 内呈良好线性关系。定量限为 10.0μg/kg。目标物的加标回收率在 84.5%至 107.3%之间,相对标准偏差(RSD)小于 7.2%。加标样品进一步通过气相色谱-四极杆轨道阱高分辨率质谱(GC-Orbitrap HRMS)进行确证。该联合方法具有较高的准确性和灵敏度,适用于牛奶中林丹及其代谢物 4-氯-2-甲基苯胺残留量的测定。

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