Online-SPE-UPLC-MS/MS检测生活污水中20种毒品

Determination of 20 illicit drugs in domestic sewage using OnlineSPE-UPLC-MS/MS

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Na_(2)EDTA·2H_(2)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,20μm)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,1.8μm)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 Na_(2)EDTA·2H_(2)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,20μm),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,1.8μm)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 were 1~250 ng·L^(-1).The correlation coefficient 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.