高效液相色谱-串联质谱法测定节瓜中的烯酰吗啉和氟吡菌胺及其代谢物的残留量

Determination of Dimethomorph,Fluopicolide and Its Metabolite Residues in Chieh-qua Using High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定节瓜中烯酰吗啉和氟吡菌胺及其代谢物2,6-二氯苯甲酰胺残留量的分析方法。样品经乙腈提取、液液分配萃取净化、浓缩定容后,以Agilent EC-C8色谱柱分离,采用UPLC-MS/MS多反应监测(MRM)正离子模式测定,外标法定量。烯酰吗啉、氟吡菌胺和2,6-二氯苯甲酰胺在节瓜中的最低检测浓度均为0.05 mg·kg^-1。在0.05、0.5、5.0 mg·kg^-13个添加水平下,烯酰吗啉、氟吡菌胺和2,6-二氯苯甲酰胺在节瓜中的平均回收率分别为82%~87%、91%~94%、76%~89%,相对标准偏差分别为4.1%~5.9%、4.5%~5.2%、0.9%~9.3%。

A method of determination for dimethomorph,fluopicolide and its metabolite residues in chieh-qua by HPLC-MS/MS was established.The analytes were extracted from samples using acetonitrile,and purified based on liquid-liquid distribution,then analyzed using UPLC-MS/MS multiple reaction monitoring(MRM)mode via positive electrospray ionization with a Waters Agilent EC-C8 column as the analytical column.All the analytes were quantified by the external standard method.The determination limit was 0.05 mg·kg^-1.The results showed that the average recoveries at the fortified levels of 0.05,0.5,5.0 mg·kg^-1 were 82%~87%、91%~94%、76%~89%,and the RSD were 4.1%~5.9%、4.5%~5.2%、0.9%~9.3%,respectively.