液相色谱-串联质谱法测定肉品中氯噻啉药物残留

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

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C_(18)吸附剂净化,然后在BEH-C_(18)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。

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.