超高效液相色谱-串联质谱法测定牛奶中三氯苯哒唑及其代谢物残留量的研究

Determination of Triclabendazole and its Metabolits Residues in Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  超高效液相色谱-串联质谱  三氯苯哒唑  三氯苯唑酮  牛奶  残留

Key words:  UPLC –MS/MS  triclabendazole  ketotriclabendazole  milk  residues

摘要:

建立了牛奶中三氯苯哒唑及其代谢物三氯苯唑酮残留量的超高效液相色谱-串联质谱（UPLC-MS/MS）测定方法。样品经乙酸乙酯提取后，正己烷除脂，经超高效液相色谱仪和C18色谱柱分离，以乙腈和5mmol/L乙酸铵溶液为流动相进行梯度洗脱。加热电喷雾负离子模式（HESI—）电离，选择反应监测模式（SRM）检测，外标法定量。结果表明：三氯苯哒唑和三氯苯哒唑酮标准溶液在5～500μg/L范围内呈现良好的线性关系，r2＞0.99，方法检测限为1μg/kg，定量限为2μg/kg。三氯苯哒唑和三氯苯唑酮在2～10μg/kg添加水平范围内的回收率为72.3%～110%，批内和批间变异系数均小于13.5%。该方法具有简便快捷、灵敏度高、准确度高等优点。

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC –MS/MS) method was established for the determining of triclabendazole(TCB) and its metabolite ketotriclabendazole(KTO-TCB) in milk. The sample was extracted by ethyl acetate and purified by hexane，and then separated by a C18 column with gradient elution solvent of 5mmol/L ammonium acetate and acetonitrile.The electrospray was operated in the negative ionization mode , TCB and KTO-TCB were identified under selected reaction monitoring (SRM). The method was quantified by external standard method.The results showed good linearity of TCB and KTO-TCB in the range of 5~500μg/L with correlation coefficients(r2) above 0.99,The limit of detection was 1μg/kg,and the limit of quantification was 2μg/kg. The average recoveries of TCB and KTO-TCB at 2~10μg/kg were 72.3%~110%,and the ralative standard deviations of intra-and inter-batch were both less than 13.5%.The method is simple,rapid,sensitive and accurate.