Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology, 11/12 Narutowicza Street, 80-233 Gdańsk, Poland.
J Chromatogr A. 2013 Sep 6;1306:44-58. doi: 10.1016/j.chroma.2013.07.050. Epub 2013 Jul 17.
A new, sensitive and rapid method based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach followed by ultra high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) was developed for the determination of nineteen endocrine disruptors (EDCs) and related compounds belonging to different classes in various fish species. Matrix effect on the analytical performance was evaluated, and thus, internal sample calibration was chosen as the most appropriate approach when analyzing such complex matrices as biota. The procedure provided adequate recoveries in the range from 40% to 103% for most of the compounds, low method detection limits (MDLs) in the range from 0.002 to 3.09ng/g for fish homogenates and high accuracy <20%. The developed method was applied for the analysis of target compounds in homogenates of different fish species from four impacted Mediterranean rivers: Ebro, Llobregat, Júcar and Guadalquivir. Eleven out of the nineteen target EDCs were found at least once in fish homogenates. Llobregat was identified as the most polluted river, where high concentrations were measured in fish homogenates especially for bisphenol A (223.91±11.51ng/g). Tris (2-butoxyethyl) phosphate (TBEP), caffeine, and methyl and benzyl paraben were found in fish from the four river basins.
建立了一种基于 QuEChERS（快速、简单、廉价、有效、耐用、安全）方法的新的、灵敏且快速的方法，结合超高效液相色谱串联质谱（UHPLC-MS/MS），用于测定 19 种不同类别属于内分泌干扰物（EDCs）和相关化合物的各种鱼类。评估了基质对分析性能的影响，因此，当分析生物群等复杂基质时，选择内部样品校准是最合适的方法。该程序为大多数化合物提供了 40%至 103%的充分回收率，对于鱼匀浆，方法检测限（MDL）低至 0.002 至 3.09ng/g，准确度高<20%。该方法应用于来自四个受影响的地中海河流（埃布罗、略夫雷加特、胡卡尔和瓜达尔基维尔）的不同鱼类匀浆中目标化合物的分析。在鱼匀浆中至少发现了 19 种目标 EDC 中的 11 种。略夫雷加特被确定为污染最严重的河流，在鱼匀浆中测量到高浓度的双酚 A（223.91±11.51ng/g）。在四个流域的鱼类中发现了三（2-丁氧基乙基）磷酸酯（TBEP）、咖啡因、甲基和苄基对羟基苯甲酸酯。
