对生活污水的前处理进行优化,建立了一种在线固相萃取-超高效液相色谱-串联质谱法(Online-SPE-UPLC-MS/MS)同时测定污水中 20 种毒品及人口标记物的方法.用金属螯合剂Na2 EDTA·2H2 O处理污水后加入同位素内标,接着用滤膜过滤后,以双柱交替模式上样.用Waters Oasis HLB固相萃取柱(2.1 mm×30 mm,20 μm)进行富集浓缩后,用流动相将固相萃取柱上吸附的目标物反冲洗到Waters ACQUITY UPLC HSS T3 色谱柱(2.1 mm×100 mm,1.8 μm)上.柱温40℃,以乙腈-0.1%(体积分数)甲酸水溶液为流动相,采用梯度程序洗脱.采用电喷雾离子源正离子、多反应监测(MRM)模式定量检测.可替宁的线性范围在 20~5000 ng·L-1,其余 20 种物质的线性范围在 1~250 ng·L-1 之间,相关系数R2 均大于 0.99,检出限在 0.01~0.25 ng·L-1 之间,加标回收率在 91.57%~113.94%,精密度均小于 15%.基于Online-SPE-UPLC-MS/MS建立了同时测定污水中 20 种毒品及人口标记物方法,该方法操作简单、灵敏高,具有良好的准确度和精密度,已成功应用于城市污水中的毒品检测,用于监测毒品滥用情况.
An online solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry(Online-SPE-UPLC-MS/MS)method was established for the simultaneous determination of 20 illicit drugs and population marker in sewage by optimizing pretreatment of sewage.Firstly,the sewage was treated with metal chelating agent Na2 EDTA·2H2 O,then the isotope in-ternal standard was added,and then the sample was loaded in two SPE columns alternating mode after being filtered by a filter mem-brane.After enrichment and concentration with Waters Oasis HLB SPE column(2.1 mm×30 mm,20 μm),the illicit drugs in sew-age adsorbed on the SPE column was backwashed to Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm)with mobile phase.The gradient elution was carried out using water(containing 0.1%formic acid,volum fraction)-acetonitrile as the mo-bile phase.The column temperature was 40℃.The electrospray positive ion source(ESI+)mode and the multiple reaction monitoring mode(MRM)were used for quantification.The linear range of cotinine was 20~5000 ng·L-1,and the linear range of the other 20 substances were1~250ng·L-1.Thecorrelationcoefficient R2 was greater than 0.99,the detection limit was 0.01~0.25 ng·L-1,the spiked recovery rate was 91.57%~113.94%and the precision was less than 15%.Based on Online-SPE-UPLC-MS/MS,a method for simultaneous determination of 20 kinds of drugs and population marker in sewage was established.This method was sim-ple,sensitive,accurate and precise.It has been successfully applied to drug detection in urban sewage for monitoring drug abuse.