Department of Chemistry, Université de Montréal, C.P. 6128, succ. Centre-Ville, Montreal, QC H3C 3J7, Canada.
J Chromatogr A. 2009 Nov 27;1216(48):8518-27. doi: 10.1016/j.chroma.2009.10.015. Epub 2009 Oct 12.
We describe the development and validation of an on-line solid-phase extraction of large-volume injections coupled to liquid chromatography-tandem mass spectrometry method for the simultaneous quantitation and confirmation of 14 selected trace organic contaminants in drinking and surface water. Selected compounds were: anti-infectives (clarithromycin, sulfamethoxazole and trimethoprim), an anticonvulsant (carbamazepine) and its transformation product 10,11-dihydrocarbamazepine, an antihypertensive (enalapril), antineoplastics (cyclophosphamide and methotrexate), herbicides (atrazine, cyanazine, and simazine) and two of their transformation products (deethylatrazine and deisopropylatrazine) and an antiseptic (triclocarban). The breakthrough volume determinations showed that out of all the investigated sorbents, the Strata-X on-line solid-phase extraction column showed the best performance. The method used a load volume of 10.0 mL and was validated using the corresponding matrices, yielding for most compounds, R(2)>0.99. Extraction recoveries ranged from 60 to 109%. The intra- and inter-day precision were <14 and <16%, respectively. The method detection limits ranged from 0.6 to 6 ng L(-1). Matrix effects were in general low. The performance of the on-line method was demonstrated with the analysis of real water samples. The application of alternative techniques of confirmation was also explored using accurate mass measurements on a time-of-flight mass spectrometer and the data-dependent reverse energy ramp scan on a triple quadrupole.
我们描述了一种在线固相萃取大体积进样结合液相色谱-串联质谱法的开发和验证,用于同时定量和确证饮用水和地表水中的 14 种选定痕量有机污染物。所选化合物为:抗感染药(克拉霉素、磺胺甲恶唑和甲氧苄啶)、抗惊厥药(卡马西平)及其转化产物 10,11-二氢卡马西平、抗高血压药(依那普利)、抗肿瘤药(环磷酰胺和甲氨蝶呤)、除草剂(莠去津、氰草津和西玛津)和它们的两种转化产物(去乙基莠去津和去异丙基莠去津)以及一种防腐剂(三氯生)。穿透体积测定表明,在所研究的所有吸附剂中,Strata-X 在线固相萃取柱表现出最佳性能。该方法采用 10.0 mL 的加载体积,并使用相应的基质进行验证,对于大多数化合物,R(2)>0.99。萃取回收率在 60%至 109%之间。日内和日间精密度分别小于 14%和 16%。方法检测限范围为 0.6 至 6ng/L。基质效应通常较低。该在线方法的性能通过对实际水样的分析得到了证明。还探索了使用飞行时间质谱仪上的精确质量测量和三重四极杆上的数据相关反向能量斜坡扫描等替代确证技术。