Center for Marine Environmental Studies (CMES), Ehime University, Bunkyo-cho 2-5, Matsuyama 790-8577, Japan.
J Chromatogr A. 2011 Jun 3;1218(22):3511-20. doi: 10.1016/j.chroma.2011.04.006. Epub 2011 Apr 12.
A multiresidue analytical method for the determination of emerging pollutants belonging to personal care products (PCPs) (antimicrobials, preservatives), benzotriazole UV stabilizers (BUVSs) and organophosphorus compounds (OPCs) in fish has been developed using high speed solvent extraction (HSSE) followed by silica gel clean up and ultra fast liquid chromatography coupled with tandem mass spectrometry (UFLC-MS/MS) analysis. Developed extraction and clean up method yielded good recovery (> 70%) for all the four groups of emerging pollutants, i.e. antimicrobials (78.5-85.6%), preservatives (85.0-89.4%), BUVSs (70.9-112%) and OPCs (81.6-114%; except for TEP - 68.9% and TPeP - 58.1%) with RSDs ranging from 0.7 to 15.4%. Intra- and inter-day repeatabilities were less than 19.8% and 19.0%, respectively at three spiked levels. The concentrations were given in lipid weight (lw) basis, and the method detection limits were achieved in the lowest range of 0.001-0.006 ng g⁻¹ for two antimicrobials, 0.001-0.015 ng g⁻¹ for four preservatives, 0.0002-0.009 ng g⁻¹ for eight BUVSs and 0.001-0.014 ng g⁻¹ for nine OPCs. Finally, the method was successfully validated as a simple and fast extraction method for the determination of 23 compounds belonging to PCPs, BUVSs and OPCs and applied to the analysis of three species of fish from Manila Bay, the Philippines. Concentrations ranged from 27 to 278 ng g⁻¹ for antimicrobials, 6.61 to 1580 ng g⁻¹ for paraben preservatives, <MDL (method detection limit) to 179 ng g⁻¹ for BUVSs and ND (not detected) to 266 ng g⁻¹ for OPCs suggesting the ubiquitous contamination by these emerging pollutants in Manila Bay. This is the first method developed for the determination of triclocarban, four paraben preservatives and four BUVSs, in fish.
一种用于测定鱼中属于个人护理产品（PCPs）（抗菌剂、防腐剂）、苯并三唑紫外线稳定剂（BUVSs）和有机磷化合物（OPCs）的新兴污染物的多残留分析方法已经开发出来，该方法使用高速溶剂萃取（HSSE），然后进行硅胶净化和超快速液相色谱-串联质谱（UFLC-MS/MS）分析。所开发的提取和净化方法对所有四组新兴污染物（即抗菌剂（78.5-85.6%）、防腐剂（85.0-89.4%）、BUVSs（70.9-112%）和 OPCs（81.6-114%；除 TEP-68.9%和 TPeP-58.1%）的回收率均>70%，相对标准偏差（RSD）范围为 0.7-15.4%。在三个加标水平下，日内和日间重复性分别小于 19.8%和 19.0%。浓度以脂重（lw）为基础给出，方法检测限在最低范围内为 0.001-0.006ng g⁻¹，两种抗菌剂，0.001-0.015ng g⁻¹，四种防腐剂，0.0002-0.009ng g⁻¹，八种 BUVSs 和 0.001-0.014ng g⁻¹，九种 OPCs。最后，该方法成功验证为一种简单快速的提取方法，用于测定来自菲律宾马尼拉湾的三种鱼类中属于 PCPs、BUVSs 和 OPCs 的 23 种化合物。抗菌剂浓度范围为 27-278ng g⁻¹，对羟基苯甲酸酯防腐剂浓度范围为 6.61-1580ng g⁻¹，<MDL（方法检测限）至 179ng g⁻¹，BUVSs 浓度范围为 ND（未检出）至 266ng g⁻¹，OPCs 表明这些新兴污染物在马尼拉湾普遍存在。这是首次开发用于测定鱼中三氯生、四种对羟基苯甲酸酯防腐剂和四种 BUVSs 的方法。
