应用化学
應用化學
응용화학
CHINESE JOURNAL OF APPLIED CHEMISTRY
2009年
10期
1222-1226
,共5页
梁华正%杨水平%郇延富%张燮%陈焕文%刘清%刘清珺%郑健
樑華正%楊水平%郇延富%張燮%陳煥文%劉清%劉清珺%鄭健
량화정%양수평%순연부%장섭%진환문%류청%류청군%정건
表面解吸常压化学电离质谱%氨基甲酸酯%快速检测
錶麵解吸常壓化學電離質譜%氨基甲痠酯%快速檢測
표면해흡상압화학전리질보%안기갑산지%쾌속검측
surface desorption atmospheric chemical ionization mass spectrometry%carbamate pesticide%rapid analysis
采用自行研制的表面解吸常压化学电离源(SDAPCI),样品未经预处理用质谱法直接测定了克百威、灭多威和异丙威3种氨基甲酸酯农药在蔬菜表面的残留,并用串联质谱法对所获得的信号离子进行结构鉴定,排除了检测结果的假阳性. 结果表明,克百威和灭多威分别形成m/z 222和m/z 163的质子化的分子离子信号,异丙威形成m/z 193的自由基阳离子信号. 串联质谱实验表明,3种氨基甲酸酯农药分子的裂解规律与其分子结构相吻合. 表面解吸常压化学电离质谱法对待测样品无污染,方法检测限低于1.0×10~(-14) g/cm~2,单个样品的测定时间平均少于1 s,特别适合于对批量样品进行快速检测.
採用自行研製的錶麵解吸常壓化學電離源(SDAPCI),樣品未經預處理用質譜法直接測定瞭剋百威、滅多威和異丙威3種氨基甲痠酯農藥在蔬菜錶麵的殘留,併用串聯質譜法對所穫得的信號離子進行結構鑒定,排除瞭檢測結果的假暘性. 結果錶明,剋百威和滅多威分彆形成m/z 222和m/z 163的質子化的分子離子信號,異丙威形成m/z 193的自由基暘離子信號. 串聯質譜實驗錶明,3種氨基甲痠酯農藥分子的裂解規律與其分子結構相吻閤. 錶麵解吸常壓化學電離質譜法對待測樣品無汙染,方法檢測限低于1.0×10~(-14) g/cm~2,單箇樣品的測定時間平均少于1 s,特彆適閤于對批量樣品進行快速檢測.
채용자행연제적표면해흡상압화학전리원(SDAPCI),양품미경예처리용질보법직접측정료극백위、멸다위화이병위3충안기갑산지농약재소채표면적잔류,병용천련질보법대소획득적신호리자진행결구감정,배제료검측결과적가양성. 결과표명,극백위화멸다위분별형성m/z 222화m/z 163적질자화적분자리자신호,이병위형성m/z 193적자유기양리자신호. 천련질보실험표명,3충안기갑산지농약분자적렬해규률여기분자결구상문합. 표면해흡상압화학전리질보법대대측양품무오염,방법검측한저우1.0×10~(-14) g/cm~2,단개양품적측정시간평균소우1 s,특별괄합우대비량양품진행쾌속검측.
Surface desorption atmospheric chemical ionization mass spectrometry(SDAPCI-MS) was used to directly determine pesticide residue on the surface of vegetables without any toxic chemical contamination. Three carbamate pesticides, carbofuran, isoprocarb and methomyl, were determined, and the structure of the molecular ions of each analyte was confirmed by collision-induced dissociation(CID) to exclude the fake positive conclusion. The results show that the carbofuran and methomyl exhibit protonated molecular ion signals at m/z 222 and m/z 163 respectively, but the isoprocarb displays free radical cation signal at m/z 193 under these conditions. The tandem mass spectrometry shows that the fragmentation regularity of the three carbamate pesticides coincide with their molecular structures. The detection limit of this method was found to be less than 1.0×10~-14 g/cm~2, and the detection time less than 1 s. SDAPCI-MS is a good method to inspect bulk samples nondestructively without sample pretreatment.