摘要
建立了超高效液相色谱-串联质谱法同时测定水果中吡菌磷、伏杀硫磷、乙硫磷、甲基嘧啶磷、速灭磷、杀扑磷、亚胺硫磷、二嗪磷、治螟磷等9种有机磷农药残留量的方法,对提取条件、流动相比例、质谱条件进行了研究。待测样品直接用含1%冰乙酸的乙腈提取,乙二胺-N-丙基硅烷(PSA)吸附剂除杂,采用电喷雾离子源(ESI)、多反应监测正离子模式扫描,外标法定量。吡菌磷等9种农药在1～18ng/mL范围内浓度与峰面积呈良好的线性关系,方法的检出限为0.005 mg/kg,添加平均回收率为79.6%～108.7%,相对标准偏差为2.0%～9.8%。方法可用于水果中吡菌磷等9种有机磷农药残留量的定量和在线定性检测。
An ultra performance liquid chromatography tandem mass spectrometric method was established for the simultaneous determination of nine organophosphorus pesticides,including pyrazophos,phosalone,ethion,pirimiphos methyl,mevinphos,methidathion,phosmet,diazinon,sulfotep,in fruits.The effect of extration condition,mobile phase,and tandem mass spectrometric parameters were investigated.The sample was extracted with acetonitrile containing 1% glacial acetic acid.And PSA was used for cleaning-up.Then the analysis was carried out under the multiple reaction monitoring（MRM） mode by employing external method.The calibration curve was linear in the range of 1~18 ng/mL.The limits of detection（LOD） for the nine pesticides was 0.005 mg/kg.The average recoveries and the relative standard derivation（RSDs） of the nine pesticides were in the range of 79.6%~108.7% and 2.0%~9.8% respectively when the spiked levels was 0.005 mg/kg,0.010 mg/kg and 0.020 mg/kg.The method could be used for simultaneous quantitative determination of pyrazophos,phosalone,ethion,pirimiphos methyl,mevinphos,methidathion,phosmet,diazinon,sulfotep in fruits.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第10期88-91,共4页
Chinese Journal of Analysis Laboratory
关键词
有机磷农药残留
超高效液相色谱-串联质谱
水果
Organophosphorus pesticide residue
Ultra performance liquid chromatography tandem mass spectrometry
Fruits
