中性解吸电喷雾萃取电离质谱法直接检测蜂蜜中的敌敌畏  

Direct Detection of Dichlorvos in Honey by Neutral DesorptionExtractive Electrospray Ionization Mass Spectrometry

作　　者：于腾辉 刘星星[1,2] 邓敏[1] 方小伟[2] 陈林飞[2] 郭夏丽[1] 罗丽萍[1] 

机构地区：[1]南昌大学,生命科学学院,南昌330031 [2]东华理工大学,江西省质谱科学与仪器重点实验室,南昌330013

出　　处：《分析化学》2016年第9期1432-1436,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.31370384);江西省科技厅项目(No.20121BDH80020);“十二五”国家科技计划课题(No.2012BDA29B01)资助~~

摘　　要：采用中性解吸电喷雾萃取电离质谱(ND-EESI-MS)技术,在无需样品预处理的条件下,建立了对蜂蜜中敌敌畏直接快速检测的方法。在正离子模式下,敌敌畏质子化离子峰位于m/z 223,二级特征离子为m/z 109和127。在优化的条件下,以m/z 127的信号强度为定量指标,建立了蜂蜜中敌敌畏残留的定量检测方法。结果表明,在蜂蜜基质中,敌敌畏在5~1000 ng/m L浓度范围内与m/z 127的信号强度线性关系良好,相关系数为0.998,检出限为1.0 ng/m L(S/N=3);蜂蜜中3个加标水平(10,30和400 ng/m L)的敌敌畏的回收率为93.0%~103.0%,精密度(RSDs)小于4.4%。同时采用气相色谱(火焰光度检测器)方法作为对照方法,检测敌敌畏加标蜂蜜样品,结果表明,加标蜂蜜在5~1000 ng/m L浓度范围内与峰面积线性关系良好,相关系数为0.999,检出限为1.6 ng/m L;10,30和400 ng/m L 3个水平加标蜂蜜的回收率为94.9%~110.3%,精密度小于7.6%。In this study,a neutral desorption-extractive electrospray ionization mass spectrometry（ ND-EESIMS） method was developed for the direct and rapid detection of dichlorvos（ DDVP） in honey samples without any sample pretreatment procedure. Under the positive ionization mode,the main characteristic parent ion of DDVP was m / z 223（ MW： 222） and daughter ions were m/z 109 and m/z127. Under the optimized working conditions,with the signal intensity of m / z 127 as quantitative index,the quantitative information of DDVP residues in honey was acquired effectively. The results showed that the linear range of DDVP for spiked honey was 5-1000 ng / m L（ R^2= 0.998） with the limit of detection（ LOD） of 1.0 ng / m L（ n = 3） and the recoveries for the DDVP spiked honey samples at the concentration levels of 10,30 and 400 ng / m L were 93. 0%-103.0%,with the relative standard deviations（ RSDs,n = 6） of less than 4.4%. Meanwhile,for detection of spiked honey with gas chromatography-flame photometric detector（ GC-FPD）,the linear range was 5-1000 ng / m L（ R^2= 0.999） with the LOD of 1. 6 ng / m L（ n = 3）,and the recoveries of DDVP at the spiked honey concentration levels of 10,30 and 400 ng / m L were 94.9%-110.3%,with the RSDs of less than 7.6%.

关 键 词：中性解吸电喷雾萃取电离 质谱 敌敌畏 蜂蜜 直接检测 

分 类 号：O657.63[理学—分析化学] S896.1[理学—化学]