液相色谱串联质谱法快速测定动物组织中克百威和其代谢产物残留量.docVIP

液相色谱串联质谱法快速测定动物组织中克百威及其代谢产物残留量 　　摘 要：建立快速测定动物组织中克百威及其代谢产物三羟基克百威残留量的液相色谱串联质谱（liquid chromatography with tandem mass spectrometry，LC-MS/MS）分析方法。动物组织样品中残留物利用乙腈提取，提取后溶液经N-丙基乙二胺（primary secondary amine，PSA）和C18材料净化，净化后的提取液经氮吹后用0.1%甲酸溶液-乙腈（50∶50，V/V）溶解，进行LC-MS/MS分析。采用Acquity BEH C18色谱柱分离，用0.1%甲酸溶液-乙腈作为流动相进行梯度洗脱，电喷雾正离子（ESI+）模式电离，多反应监测（multiple reaction monitoring，MRM）模式检测，内标法定量。克百威和三羟基克百威分别在0.05～25.0 μg/L和0.25～50.0 μg/L质量浓度范围内具有良好的线性关系，线性相关系数均大于0.999；在动物组织（猪肉和牛肉）中克百威和三羟基克百威的方法检测限分别为0.10 μg/kg和0.50 μg/kg，定量限分别为0.25 μg/kg和1.0 μg/kg。添加范围为0.25～10 μg/kg时，平均回收率在95.7%～107.0%之间，批内相对标准偏差（relative standard deviation，RSD）在3.2%～5.9%之间，批间RSD在4.5%～6.6%之间。该方法能满足动物肉组织中克百威及其代谢产物残留量快速分析的要求 关键词：动物组织；克百威；三羟基克百威；快速测定；液相色谱串联质谱法；残留量 Fast Determination of Residues of Carbofuran and Its Metabolite in Animal Tissues by Liquid Chromatography with Tandem Mass Spectrometry YANG Ting， L? Yan， CHEN Guo， WU Yinliang* （The Ningbo Academy of Agricultural Sciences， Ningbo 315040， China） Abstract： A method for determining residues of carbofuran and its metabolite 3-hydroxycarbofuran in animal tissues was developed by liquid chromatography with tandem mass spectrometry. Samples were extracted with acetonitrile. Then the extract was purified by dispersive solid phase extraction method using PSA and C18 as sorbents. After purification， the extract was dried under nitrogen stream and the residue was dissolved in 0.1% formic acid solution/acetonitrile mixture （50/50， V/V） and filtered through a 0.22 ?m filter and 10 ?L of the filtrate was injected into the LC system for analysis. The analysis was performed on an Acquity BEH C18 column with a mixture of 0.1% formic acid solution and acetonitrile as the mobile phase under gradient elution conditions. The mass spectrometer was operated in multiple reaction monitoring （MRM） mode with positive ion electrospray ionization （ESI）. The analytes were quantified with the isotope internal standard dilution method. Good linearity was obtained for carbofura