超高效液相色谱-串联质谱法测定菠菜、苹果及大豆中二硝基苯胺类除草剂残留量  

Simultaneous Determination of Dinitroaniline Herbicides in Spinach,Apple and Soybean by UPLC-MS/MS

作　　者：张建莹[1] 靳保辉[1] 吴卫东[1] 邓慧芬[1] 林珊[1] 梁淑雯[1] ZHANG Jianying;JIN Baohui;WU Weidong;DENG Huifen;LIN Shan;LIANG Shuwen(Shenzhen Exit Entry Inspection & Quarantine Bureau,Shenzhen518045,China)

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518045

出　　处：《质谱学报》2018年第1期69-75,共7页Journal of Chinese Mass Spectrometry Society

基　　金：国家质检总局项目(2016IK240)资助

摘　　要：以菠菜、苹果和大豆为代表性分析物,建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)检测蔬菜、水果及粮谷等植物源性食品中8种二硝基苯胺类除草剂(氟乐灵、二甲戊乐灵、仲丁灵、异乐灵、磺乐灵、氨基乙氟灵、氨磺乐灵和氨基丙氟灵)的残留量。采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测,并使用外标法定量。结果表明:8种二硝基苯胺类除草剂的测定低限均为10μg/kg;在添加水平10~200μg/kg范围内,加标回收率为70.0%~120%,相对标准偏差为0.56%~23.0%。该方法灵敏、有效,适用于蔬菜、水果和粮谷等植物源性食品中二硝基苯胺类除草剂多残留的测定。A method of ultra performance liquid chromatography tandem mass spectrometry(UPLC MS/MS)was developed for determination of8kinds of dinitroaniline herbicides(trifluralin,pendimethalin,butralin,isopropalin,dinitramine,nitralin,oryzalin,prodiamine)in spinach,apple and soybean.Afer homogenization,5.0g sample was soaked with7mL water for1h.Then3g NaCl was added,and the sample was extracted twice by25mL hexane saturated acetonitrile solution.After concentration,the extract was put through C18column and eluted by5mL acetonitrile.The eluated was then concentrated and dissolved with2.0mL hexane acetone mixture(2∶8,V/V).The preparation was cleaned by Envi Carb column and eluted with5.0mL hexane acetone.The residue was dissolved by50%acetonitrile aqueous solution(contain0.1%formic acid),and determined by UPLC ESI/MS/MS.Under the optimized chromatographic conditions,8target compounds were obtained.Confirmation was achieved using electro spray ionization(ESI)in positive mode with multiple reaction monitoring(MRM),and external standard method was used for quantification.The results show that8dinitroaniline herbicides have good linearity,the linearity is more than0.99.The limits of quantification(LOQs)are10μg/kg.The mean recoveries are between70.0%and120%at the spiked levels of10-200μg/kg.The RSD of the method are between0.56%and23.0%.The method is precise,sensitive and accurate,which is suitable for confirmation and quantification of dinitroaniline herbicides in vegetables,fruits and grains.

关 键 词：超高效液相色谱-串联质谱(UPLCMS/MS) 二硝基苯胺 除草剂 蔬菜 水果 粮谷 

分 类 号：O657.63[理学—分析化学]