快速高分离液相色谱-串联质谱法测定水产品中敌百虫残留

Determination of trichlorphon residues in aquatic product by RRLC-MS/MS

目的:建立快速高分离液相-串联质谱法(RRLC-MS/MS)测定水产品中敌百虫的残留量。方法:样品用酸化乙酸乙酯提取,酸性氧化铝柱净化,旋转蒸发减压蒸干后,用流动相溶解,高分离度快速液相色谱分离,电喷雾串联四级杆质谱进行检测,外标法定量。结果:本法敌百虫在0.1 ng/ml～20 ng/ml的范围内线性关系良好,r=1.0000,在0.5μg/kg～5μg/kg的3个添加水平的平均回收率为90.44%～109.46%,相对标准偏差为3.45%～6.21%。方法检测限0.5μg/kg。结论:本法在3.5 min内快速完成分析测试,可应用于大通量的实际样品检测。

Objective：To establish a method for the determination of the residues of trichlorphon in aquatic products by rapid high resolution liquid chromatography coupled with tandem mass spectrum（RRLC-MS/MS）.Methods：The samples were extracted with acidified acetic ether and the extracts were purified with acidic alumina column,dried by rotary evaporator,and dissolved in the mobile phase.The sample was determined by RRLC-MS/MS,and quantified by external standard method.Results：The linear range of the method was 0.1 ng/ml～20 ng/ml,r=1.0000.At three levels（0.5 μg/kg,1.0 μg/kg and 5.0 μg/kg）,the average recoveries were 90.44%～109.46%,and relative standard deviations were 3.45%～6.21%,the limit of detection was 0.5 μg/kg.Conclusion：The method could be quickly finished in 3.5 min and applied to the analysis of batch samples.