高效液相色谱-串联质谱法测定茶叶、三七中胺苯磺隆和甲基胺苯磺隆的残留量  

Determination of residues of Ethametsulfuron and Ethametsulfuron-methyl in Tea and Panax Notoginseng by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：魏一婷 WEI Yiting(Xiamen Customs Technology Center,Xiamen 361013;Xu Dunming Employee Innovation Studio,Xiamen 361013)

机构地区：[1]厦门海关技术中心,福建厦门361013 [2]徐敦明职工技术创新工作室,福建厦门361013

出　　处：《分析科学学报》2023年第4期492-496,共5页Journal of Analytical Science

基　　金：云南省科技厅科技计划项目(202102AE090042)。

摘　　要：建立了测定茶叶、三七中胺苯磺隆和甲基胺苯磺隆残留量的高效液相色谱-串联质谱法。样品经超纯水浸泡,乙腈提取,QuEChERS净化,Phenomenex Kinetex C 18色谱柱(50×2.1 mm,2.6μm)分离,液相色谱-串联质谱法检测,基质匹配外标法定量。胺苯磺隆和甲基胺苯磺隆在1.0 ng/mL~100 ng/mL范围内线性关系良好,相关系数R均大于0.999,方法的检出限(S/N=3)为0.07μg/kg~0.20μg/kg,定量限(S/N=10)为0.21μg/kg~0.60μg/kg。在5μg/kg~100μg/kg范围的回收实验中,胺苯磺隆平均回收率为70.8%~108.1%,相对标准偏差(RSD,n=6)为3.3%~11.4%;甲基胺苯磺隆平均回收率为70.2%~105.5%,RSD(n=6)为2.9%~10.6%。本方法前处理简单、稳定、灵敏,适用于茶叶、三七中胺苯磺隆和甲基胺苯磺隆残留量的同时测定。A method was established for simultaneous determination of ethametsulfuron and ethametsulfuron-methyl residues in tea and panax notoginseng by high performance liquid chromatography-tandem mass spectrometry.The sample was soaked in ultrapure water,extracted with acetonitrile,purified by QuEChERS,separated on a Phenomenex Kinetex C 18 chromatographic column(2.6μm,50×2.1 mm),detected by liquid chromatography tandem mass spectrometry,and quantified by matrix matching external standard method.Good linearity was obtained in the range of 1.0 ng/mL^(-1)00 ng/mL with correlation coefficients(R^(2))≥0.9990.The limits of detection(LODS,S/N≥3)were 0.07μg/kg-0.20μg/kg and the limits of quantification(LOQS,S/N≥10)were 0.21μg/kg-0.60μg/kg.When the spiking concentration were 5μg/kg-100μg/kg,the average recovery rate of Ethametsulfuron were 70.8%-108.1%with the relative standard deviation(n=6)of 3.3%-11.4%,and the average recovery rate of Ethametsulfuron-methyl were 70.2%-105.5%with the relative standard deviation(n=6)of 2.9%-10.6%.The method is simple,sensitive and stable,which is suitable for the simultaneous determination of ethametsulfuron and ethametsulfuron-methyl residues in tea and panax notoginseng.

关 键 词：茶叶 三七 胺苯磺隆 甲基胺苯磺隆 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]