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：
在这里，采用气相色谱-串联质谱法(GC-MS/MS)首次测定了牛奶中的氯丁虫及其代谢产物4-氯-2-甲基苯胺残留量。样品用乙腈提取,用快速清洗，easy,便宜,有效,崎岖,和安全（QuEChERS）方法。使用DB-17MS柱进行分离。在选定的反应监测（SRM）模式下进行检测，并使用基质匹配的同位素内标方法进行定量。在最优条件下,在10-200µg/kg的浓度范围内观察到良好的线性关系。定量限为10.0µg/kg。目标物质的加标回收率为84.5%至107.3%，相对标准偏差(RSD)<7.2%。通过气相色谱-四极杆-Orbitrap高分辨率质谱(GC-OrbitrapHRMS)进一步确认加标样品。该方法准确度高,灵敏度高,适用于牛奶中杀虫脒及其代谢产物4-氯-2-甲基苯胺残留量的测定。
