摘要
建立了超高效液相色谱-串联质谱法(UPLC-MS/MS),可于10min内快速测定土壤中的239种农药残留。土壤样品经AOAC(Association of Official Analytical Chemists)QuEChERS方法处理,用乙腈萃取;无水硫酸镁、乙酸钠固液分离后,过0.2μm滤膜;在UPLC-MS/MS正、负离子同步扫描多反应监测模式下进行分析。239种农药中,线性相关系数(r2)大于0.99的有236个,占总数的99%。在40μg/kg添加水平下所有被检测农药的回收率均在50%～150%之间,且相对标准偏差(RSD)均小于20%;其中有209种农药的回收率达到70%～120%,有161种的RSD小于10%。方法的检出限(LOD)范围为0.69～29.04μg/kg。土壤中多种农药残留的同时检测要求时间短、准确度和精密度高,本方法符合这些检测要求,适用于土壤中农药残留的检测。
A method for the determination of 239 pesticides in soil samples by ultra perform- ance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） is presented. The sam- ple was prepared with AOAC （Association of Official Analytical Chemists） QuEChERS method for the extraction （acetonitrile, anhydrous MgSO4, CH^COONa）. After filtered with a 0.2 ~m membrane, the sample was separated and detected by UPLC-MS/MS performing on positive/ negative electrospray ionization （ESI ＋/- ） and the multiple reaction monitoring （MRM） mode. In this study, 236 of the 239 pesticides＇ correlation coefficients were above 0.99, which counted 99% of all the analytes. The limits of detection （LODs） ranged in 0.69 -29.04 ~g/kg （S/N = 3）. The recoveries of all the pesticides at 40 ~g/kg spiked level were in the range of 50%- 150%, and the relative standard deviations （RSDs） were below 20%. In addition, the recoveries of 209 pesticides were in the range of 70% - 120%, and RSDs of 161 pesticides were less than 10%. The method is efficient, fast, simple, and accurate. The procedure is suitable for the determination of multi pesticide residues in soil.
出处
《色谱》
CAS
CSCD
北大核心
2013年第9期850-861,共12页
Chinese Journal of Chromatography
基金
青岛市公共领域科技支撑计划项目(11-2-3-55-nsh)
青岛农业大学高层次人才基金(630608)
关键词
QUECHERS
超高效液相色谱-串联质谱法
农药
多残留
土壤
QuEChERS
ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）
pesticides
multi-residues
soil
