液相色谱-串联质谱法测定肉品中氯噻啉药物残留

采用液相色谱-串联质谱（liquid chromatography-tandem mass spectrometry，LC-MS/MS）法测定肉 品中氯噻啉药物残留。肉样经过酸化乙腈提取后，采用N-丙基乙二胺和C18吸附剂净化，然后在BEH-C18柱 （2.1 mm×50 mm，1.7 μm）上用乙腈和体积分数为0.1%的甲酸水溶液为流动相进行梯度洗脱，流速0.30 mL/min。 样品经电喷雾离子源正离子模式电离后，在多反应监测模式下定性及定量。结果表明：该方法在10～400 ng/mL范 围内线性关系良好，方法检出限为5.0 μg/kg，回收率为91.41%～93.51%，相对标准偏差在2.4%～3.2%之间。该方 法结合了QuEChERS（quick，easy，cheap，effective，rugged，safty）和LC-MS/MS的优点，操作简便、分析速度 快、灵敏度高、重现性好，可以用于肉品中氯噻啉残留的检测。

Determination of Imidaclothiz Residues in Meat by Liquid Chromatography-Tandem Mass Spectrometry

This paper presents a method for the determination of imidaclothiz residue in meat by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted with acidic acetonitrile, and the extract was then cleaned up with primary secondary amine (PSA) and C18 sorbent. The separation was performed on a BEH-C18 column (2.1 mm × 50 mm, 1.7 μm) using gradient elution with acetonitrile and 0.1% formic acid in water as mobile phase at a flow rate of 0.30 mL/min. The analyte was detected with an electrospray ionization source in the positive ion mode (ESI+) using multiple reaction monitoring (MRM). The results showed that the developed method exhibited good linearity over the concentration range of 10–400 ng/mL. The limit of detection was 5.0 μg/kg, and the recovery was 91.41%–93.51% with relative standard deviation between 2.4% and 3.2%. This method, combining the advantages of both QuEChERS (quick, easy, cheap, effective, rugged, safty) and LC-MS/MS such as simplicity, rapidity, high sensitivity, and good reproducibility, can be used for the determination of imidaclothiz residue in meat.