Segura Pedro A, Gagnon Christian, Sauvé Sébastien
Département de Chimie, Université de Montréal, C.P. 6128, Succursale Centre-Ville, Montréal, QC, Canada H3C 3J7.
Anal Chim Acta. 2007 Dec 5;604(2):147-57. doi: 10.1016/j.aca.2007.09.058. Epub 2007 Oct 9.
We developed and validated a novel on-line preconcentration liquid chromatography-tandem mass spectrometry method for the determination of anti-infectives in wastewaters. The presented method preconcentrates 1 mL of sample in a load column using a switching-valve technique. The method was optimized with respect to sample load flow rate, volume of the load column wash and organic solvent content of the load column wash. The sample is cleaned using a 30% organic solvent washing step and then gradually eluted to an analytical column for separation. To compensate for matrix effects, quantitation was performed using standard additions. Confirmation of the presence of the detected compounds was done using a second selective reaction monitoring transition. Method intra-day precision was less than 9% and inter-day precision %R.S.D. varied between 2.5 and 23%. Limits of detection for the selected anti-infective compounds ranged from 13 to 61 ng L(-1). All the target anti-infectives were found in the city of Montréal WWTP effluent in concentrations ranging from 71 to 289 ng L(-1). This automated method eases the rapid quantitation of those trace contaminants using small sample volumes.
我们开发并验证了一种用于测定废水中抗感染药物的新型在线预浓缩液相色谱 - 串联质谱法。所提出的方法采用切换阀技术在加载柱中对1 mL样品进行预浓缩。该方法针对样品加载流速、加载柱洗涤体积和加载柱洗涤液的有机溶剂含量进行了优化。样品通过30%有机溶剂洗涤步骤进行净化，然后逐步洗脱至分析柱进行分离。为补偿基质效应，采用标准加入法进行定量。使用第二个选择性反应监测跃迁对检测到的化合物的存在进行确认。方法日内精密度小于9%，日间精密度%R.S.D.在2.5%至23%之间变化。所选抗感染化合物的检测限范围为13至61 ng L⁻¹。在蒙特利尔市污水处理厂的出水中发现所有目标抗感染药物的浓度范围为71至289 ng L⁻¹。这种自动化方法使用少量样品体积便于对那些痕量污染物进行快速定量。
