超高效液相色谱-串联质谱法测定热带水果中杀虫双残留

Determination of bisultap residue in tropical fruits by ultra performance liquid chromatography-tandem mass spectrometry

采用改进的QuEChERS方法,结合超高效液相色谱-串联质谱法(UPLC-MS/MS),建立了热带水果中杀虫双残留的测定方法。热带水果经含1%(v/v)乙酸的乙腈溶液二次提取,200 mg N-丙基乙二胺(PSA)、100 mg C18、300 mg MgSO4和500 mg柠檬酸氢二钠净化。采用CAPCELL CORE PC亲水色谱柱进行分离,在负离子多反应监测(MRM)模式下检测,外标法定量。结果表明,杀虫双在0. 1～10. 0μg/L范围内线性关系良好,相关系数(r2)为0. 999 3,检出限和定量限分别为0. 015μg/kg和0. 05μg/kg,加标回收率为81. 0%～88. 3%,相对标准偏差(RSD)为3. 9%～6. 2%。该法净化效果好,灵敏度高,适于热带水果中杀虫双残留的快速定性和定量分析。

A method for the determination of bisultap in tropical fruits was developed by modified QuEChERS method and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The tropical fruit samples were twice extracted with acetonitrile containing 1%(v/v)acetic acid,and purified by 200 mg of primary secondary amine(PSA),100 mg of C18,300 mg of MgSO 4 and 500 mg of disodium hydrogen citrate.The analyte was separated on a CAPCELL CORE PC hydrophilic column,detected in the negative ion multiple reaction monitoring(MRM)mode,and quantified by external standard method.A good linear relationship in the range of 0.1-10.0μg/L was obtained with the correlation coefficient(r 2)of 0.999 3.The limit of detection and limit of quantification were 0.015μg/kg and 0.05μg/kg,respectively.The spiked recoveries were in the range of 81.0%-88.3%with the relative standard deviations from 3.9%to 6.2%.The method has good purification effect and high sensitivity,and is suitable for the rapid analysis of the bisultap residues in tropical fruits.