超高效液相色谱-串联质谱法测定蔬菜和土壤中苯线磷及其代谢物残留量

Determination of Fenamiphos and its Metabolites Residues in Vegetables and Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了蔬菜和土壤中苯线磷及其代谢物苯线磷砜和苯线磷亚砜残留的分析方法。蔬菜样品用乙腈均质提取,盐析分配,提取液采用C_(18)和PSA粉末分散固相萃取净化;土壤样品用丙酮-正己烷(1+1)溶剂超声波提取,LCNH2固相萃取小柱净化,净化后的样液供超高效液相色谱-串联质谱仪(UPLC-MS/MS)分析,采用电喷雾离子化正离子方式(ESI+)及多反应监测模式(MRM)进行测定,基质匹配标准溶液外标法定量。在最优条件下进行测试,苯线磷、苯线磷砜和苯线磷亚砜的定量限(S/N≥10)为0.01 mg/kg。在加标水平为0.01 mg/kg、0.05 mg/kg和0.10 mg/kg时,回收率为81.5%~106.9%,相对标准偏差为3.4%~10.7%。

A method for the determination of fenamiphos and its metabolites residues in vegetables and soil was developed by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The vegetable samples were extracted with acetonitrile-water and separated with salting out method.And then the supernatants were purified using dispersive solid-phase extraction(C_(18) and PSA powder)prior to the UPLC-MS/MS analysis.The soil samples were extracted with Acetone-hexane(1+1)and then the supernatants were purified using LC-NH2 solid-phase extraction prior to the UPLCMS/MS analysis.The analytes were separated by HSS T3 column,indentified by positive electrospray ionization(ESI+)and multiple reaction monitoring(MRM)mode.The matrix-matched external standard calibration curves were used for quantitative analysis.Under the optimal conditions,the detection limits of the method(S/N≥10)were 0.01 mg/kg.Tests for recovery were carried by addition of standards at concentration of 0.01 mg/kg,0.05 mg/kg and 0.10 mg/kg,the results were 81.5%~106.9%,and the relative standard deviations were in the range of 3.4%~10.7%.