Catalan Institute for Water Research ICRA, Emili Grahit 101, 17003 Girona, Spain.
J Chromatogr A. 2013 May 3;1288:63-72. doi: 10.1016/j.chroma.2013.03.001. Epub 2013 Mar 13.
A new sensitive method based on pressurized liquid extraction (PLE) and purification by gel permeation chromatography (GPC) prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed for the determination in fish homogenate, liver and muscle of twenty pharmaceuticals compounds and metabolites from seven commonly used therapeutic families. An extensive matrix effect evaluation was performed in order to select the best approach when analyzing such complex matrices. Limits of detection (MDLs) for the target compounds were in the range of 0.03-0.50ng/g for fish homogenate, 0.01-0.42ng/g for fish muscle, and 0.08-0.98ng/g for fish liver. The method was applied to fish tissues of eleven fish species from four heavily impacted Mediterranean rivers. Nine compounds from five therapeutic families were measured at concentrations higher than MDLs. Highest levels were found in trout liver, with a maximum concentration of 18ng/g for carbamazepine, whereas the most ubiquitous compound was diclofenac.
建立了一种基于加压液体萃取（PLE）和凝胶渗透色谱（GPC）净化，结合超高效液相色谱-串联质谱（UHPLC-MS/MS）的新的灵敏方法，用于测定鱼匀浆、肝脏和肌肉中 20 种来自 7 种常用治疗类别的药物化合物和代谢物。为了分析如此复杂的基质，我们进行了广泛的基质效应评估，以选择最佳方法。目标化合物的检测限（MDLs）在鱼匀浆中的范围为 0.03-0.50ng/g，在鱼肌肉中的范围为 0.01-0.42ng/g，在鱼肝脏中的范围为 0.08-0.98ng/g。该方法应用于来自四个受地中海影响严重的河流的 11 种鱼类的鱼组织中。在高于 MDLs 的浓度下测量了来自五个治疗类别的 9 种化合物。在鳟鱼肝脏中发现了最高水平，卡马西平的最高浓度为 18ng/g，而最普遍的化合物是双氯芬酸。
