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  

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

作　　者：曹海微[1] 田芳洁 康明芹[1] 李荣荣[1] 杨璐[1] 顾婷婷[1] 

机构地区：[1]吉林出入境检验检疫局,吉林长春130062 [2]长春市食品药品监督管理局南关监督管理所,吉林长春130062

出　　处：《化学试剂》2017年第11期1188-1192,共5页Chemical Reagents

基　　金：国家质检总局科技资助项目(2012IK162;2013IK162)

摘　　要：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。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% and96. 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.

关 键 词：高效液相色谱-串联质谱 粮谷 十二环吗啉 十三吗啉 

分 类 号：O657.63[理学—分析化学]