高效液相色谱-串联质谱法测定蔬菜水果中双甲脒及其代谢产物  

Determination of amitraz and its metabolites in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry

作　　者：黄娟 桂茜雯 高玲 张晓燕 沈伟健 吴斌 丁涛 HUANG Juan;GUI Qianwen;GAO Ling;ZHANG Xiaoyan;SHEN Weijian;WU Bin;DING Tao(Animal,Plant and Food Inspection Center,Nanjing Customs,Nanjing 210019,China)

机构地区：[1]南京海关动植物与食品检测中心,江苏南京210019

出　　处：《色谱》2019年第1期2-7,共6页Chinese Journal of Chromatography

基　　金：政府间国际科技创新合作重点专项(2017YFE0110800)~~

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)检测蔬菜水果中双甲脒(AMZ)及其降解或代谢产物单甲脒(DMPF)、2,4-二甲基苯基甲酰胺(DMF)和2,4-二甲基苯胺(DMA)的分析方法。样品经0. 1 mol/L NaOH溶液稀释、正己烷-异丙醇(2∶1,v/v)混合提取液提取,然后采用HPLC-MS/MS对目标物进行定性确证和定量分析。采用Pheno m enex Kinetex C18色谱柱(100 m m×4. 6 m m,2. 6μm)分离,以0. 1%(v/v)甲酸水溶液和甲醇为流动相进行梯度洗脱,采用电喷雾电离(ESI)源、正离子监测模式进行检测。在1. 0～200. 0μg/L范围内,4种目标化合物呈良好的线性关系,相关系数(r)大于0. 99;方法的定量限为0. 01～0. 4μg/kg。4种目标化合物在0. 5、5. 0和20. 0μg/kg 3个水平下的加标回收率为62. 5%～105. 0%,RSD为7. 5%～17. 6%。该法简便快捷,准确可靠,灵敏度高,定量限满足目前国内外残留限量要求。A method was established for the determination of amitraz(AMZ),and its metabolites semiamitraz(DMPF),2,4-dimethylformamidine(DMF)and 2,4-dimethylaniline(DMA)in vegetables and fruits by using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were diluted with 0.1 mol/L sodium hydroxide and extracted with n-hexane-isopropanol(2∶1,v/v).The separation was performed on a Phenomenex Kinetex C18 column(100 mm×4.6 mm,2.6μm)with gradient elution using 0.1%(v/v)formic acid aqueous solution-methanol as the mobile phase.The analysis of amitraz and its metabolites were detected under electrospray positive ionization mode.The limits of quantification(LOQs)were between 0.01 and 0.4μg/kg.The good linearities(r>0.99)were achieved for the target compounds in the range of 1.0-200.0μg/L.The recoveries at three spiked levels(0.5,5.0 and 20μg/kg)in blank matrix were in the range of 62.5%-105.0%with the relative standard deviations between 7.5%and 17.6%.The method is convenient,rapid,accurate,efficient,sensitive and practical.It is suitable for the determination and confirmation of amitraz and its metabolites in vegetables and fruits,and can meet the demands of domestic and foreign regulations.

关 键 词：高效液相色谱-串联质谱 代谢产物 双甲脒 单甲脒 2 4-二甲基苯基甲酰胺 2 4-二甲基苯胺 蔬菜水果 

分 类 号：O658[理学—分析化学]