Institute for the Dynamics of Environmental Processes, National Research Council (CNR-IDPA), Via Torino 155, 30172, Venice Mestre, VE, Italy.
Department of Environmental Sciences, Informatics and Statistics, Ca' Foscari University of Venice, Via Torino 155, 30172, Venice Mestre, VE, Italy.
Anal Bioanal Chem. 2016 Nov;408(28):7991-7999. doi: 10.1007/s00216-016-9897-x. Epub 2016 Sep 10.
This study develops and validates a novel analytical approach for the simultaneous determination of 127 polychlorinated biphenyls (PCBs), together with 6 polychlorinated naphthalenes (PCNs) and 16 polycyclic aromatic hydrocarbons (PAHs). PCBs, PCNs, and PAHs were subjected to a unique pretreatment protocol and were simultaneously determined in a single chromatographic run, using GC-MS, in environmental marine samples of mussels and clams. The results of the validation experiments, which were performed on the standard reference materials (NIST SRM 1974C - slurried matrix and NIST SRM 2977 - freeze-dried matrix), were in accordance with the certified and the reference values. The repeatability of the method for all target compounds, expressed as mean relative standard deviations, ranged from 2.5 to 5.1 % for PCBs, from 3.9 to 5.5 % for PCNs, and from 8.6 to 17.9 % for PAHs; the first value of each pair refers to the freeze-dried matrix and the second to the fresh one, for each of the classes of compounds examined. The quantification limits were in the range of 0.2-6 pg for PCBs, 0.4-8 pg for PCNs, and 0.2-15 pg for PAHs (on column). The method recoveries yielded good results (62 ± 19 % for the freeze-dried matrix and 60 ± 14 % for the fresh one) and were not significantly reduced by adopting a single analytical protocol compared with the use of different group-specific analytical methods. No serious interferences were encountered and good selectivity was achieved. These results show that this method allows one to increase the laboratory sample throughput while requiring a small amount of tissue and saving time. Graphical Abstract Simultaneous determination of halogenated contaminants and polycyclic aromatic hydrocarbons: a multianalyte method applied to filter-feeding edible organisms.
本研究开发并验证了一种新颖的分析方法,用于同时测定 127 种多氯联苯(PCBs)、6 种多氯萘(PCNs)和 16 种多环芳烃(PAHs)。将 PCBs、PCNs 和 PAHs 进行独特的预处理,并在单个色谱运行中使用 GC-MS 同时测定贻贝和蛤等环境海洋样本中的这些物质。在标准参考物质(NIST SRM 1974C-浆状基质和 NIST SRM 2977-冻干基质)上进行的验证实验结果与证书值和参考值相符。对于所有目标化合物,方法的重复性(以平均相对标准偏差表示)在 2.5%至 5.1%之间,适用于 PCBs;在 3.9%至 5.5%之间,适用于 PCNs;在 8.6%至 17.9%之间,适用于 PAHs;每对中的第一个值指的是冻干基质,第二个值指的是新鲜基质,适用于所检查的化合物类别。定量限在 0.2-6pg 之间,适用于 PCBs;在 0.4-8pg 之间,适用于 PCNs;在 0.2-15pg 之间,适用于 PAHs(柱上)。该方法的回收率效果良好(对于冻干基质为 62%±19%,对于新鲜基质为 60%±14%),与采用不同组特异性分析方法相比,采用单一分析方案不会显著降低回收率。未遇到严重干扰,且选择性良好。这些结果表明,该方法可在需要少量组织和节省时间的情况下,提高实验室样品通量。