高效液相色谱-串联质谱法测定粮谷中十二环吗啉和十三吗啉残留量

建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定粮谷中十二环吗啉和十三吗啉残留量的分析方法。样品经1%甲酸-乙腈超声提取、石墨化炭黑/氨基复合固相萃取柱净化、HPLC-MS/MS多反应监测模式测定、外标法定量。结果表明,十二环吗啉和十三吗啉在2.0~200.0μg/L范围内线性关系良好,相关系数均大于0.999。本方法对十二环吗啉和十三吗啉的定量限分别为2.0和5.0μg/kg,样品基质中两种目标物在3个添加水平的平均回收率为78.0%~96.0%,相对标准偏差(RSD)为3.0%~8.2%。该方法简单、灵敏、准确、可靠,可用于粮谷中十二环吗啉和十三吗啉残留的分析。

Determination of Dodemorph and Tridemorph in Grain Using High Performance Liquid Chromatography-tandem Mass Spectrometry

High performance liquid chromatography-trandem mass spectrometry(HPLC-MS/MS) was applied to determine the dodemorph and tridemorph residues in grain.The analytes in samples were extracted using 1％ formic acid-acetonitrile mixture as the extraction solvent and were further purified with the ENVI-carb/LC cartridge.The purified liquid was detected using HPLC-MS/MS and quantified using external standard method.The results showed that the good linear range for dodemorph and tridemorph were 2.0～200.0 μg/L,and the correlation coefficients were higher than 0.999.The limit of quantification for the dodemorph and tridemorph was 2.0 and 5.0 μg/kg respectively.The recoveries of the analytes at three spiked levels ranged between 78.0％ and 96.0％ with the relative standard deviations of 3.0％ ～8.2％.The present method is simple,sensitive,reliable and accurate which can be suitible for dodemorph and tridemorph analysis of grain.