Catalan Institute for Water Research (ICRA), C/Emili Grahit 101, 17003 Girona, Spain.
J Chromatogr A. 2013 May 31;1292:173-88. doi: 10.1016/j.chroma.2012.12.072. Epub 2013 Jan 10.
The present work describes the development of a fast and robust analytical method for the determination of 53 antibiotic residues, covering various chemical groups and some of their metabolites, in environmental matrices that are considered important sources of antibiotic pollution, namely hospital and urban wastewaters, as well as in river waters. The method is based on automated off-line solid phase extraction (SPE) followed by ultra-high-performance liquid chromatography coupled to quadrupole linear ion trap tandem mass spectrometry (UHPLC-QqLIT). For unequivocal identification and confirmation, and in order to fulfill EU guidelines, two selected reaction monitoring (SRM) transitions per compound are monitored (the most intense one is used for quantification and the second one for confirmation). Quantification of target antibiotics is performed by the internal standard approach, using one isotopically labeled compound for each chemical group, in order to correct matrix effects. The main advantages of the method are automation and speed-up of sample preparation, by the reduction of extraction volumes for all matrices, the fast separation of a wide spectrum of antibiotics by using ultra-high-performance liquid chromatography, its sensitivity (limits of detection in the low ng/L range) and selectivity (due to the use of tandem mass spectrometry) The inclusion of β-lactam antibiotics (penicillins and cephalosporins), which are compounds difficult to analyze in multi-residue methods due to their instability in water matrices, and some antibiotics metabolites are other important benefits of the method developed. As part of the validation procedure, the method developed was applied to the analysis of antibiotics residues in hospital, urban influent and effluent wastewaters as well as in river water samples.
本工作描述了一种快速而稳健的分析方法的开发，用于测定环境基质中 53 种抗生素残留，涵盖了各种化学基团和它们的一些代谢物，这些环境基质被认为是抗生素污染的重要来源，即医院和城市废水，以及河水。该方法基于自动化离线固相萃取（SPE），然后进行超高效液相色谱-四极杆线性离子阱串联质谱（UHPLC-QqLIT）分析。为了进行明确的鉴定和确证，并为了满足欧盟指南的要求，对每个化合物监测两个选择反应监测（SRM）跃迁（最强烈的一个用于定量，第二个用于确证）。通过使用每个化学基团的一种同位素标记化合物进行内标法，对目标抗生素进行定量，以校正基质效应。该方法的主要优点是自动化和加速样品制备，通过减少所有基质的提取体积，通过使用超高效液相色谱快速分离广泛的抗生素，其灵敏度（在低 ng/L 范围内的检测限）和选择性（由于串联质谱的使用）。β-内酰胺类抗生素（青霉素类和头孢菌素类）的纳入是多残留方法中难以分析的化合物，因为它们在水基质中不稳定，而一些抗生素代谢物是该方法开发的其他重要优点。作为验证程序的一部分，该方法应用于分析医院、城市废水进水和出水以及河水样品中的抗生素残留。
