Simultaneous determination of halogenated contaminants and polycyclic aromatic hydrocarbons: a multi-analyte method applied to filter-feeding edible organisms

Abstract

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.

Sustainability of using vineyard pruning residues as an energy source: Combustion performances and environmental impact

“…QFFs were broken in small pieces and mixed with anhydrous sodium sulfate, diatomaceous earth and Ottawa sand (Sigma-Aldrich Co., Applied Separation Inc.). The operative conditions were previously optimized for enhanced extraction efficiency and to minimize the amount of solvent required [40,41]. The extractions were performed at 100°C and 100 bar, with 3 static cycles of 7 min each.…”

“…The eluates were collected as one single fraction. Purified samples were reduced to 100 μL under a gentle nitrogen flow at 23°C and spiked with a known amount of the recovery standard solution (1 13 C-labelled PAHs at ng μL −1 , 2 13 Clabelled PCBs at pg μL −1 and 2 13 C-labelled PCDD/Fs at 20 pg μL −1 ; CIL Inc.) according to the method fully described in Pizzini et al [41,47].…”

Simultaneous detection of chlorinated polycyclic aromatic hydrocarbons with polycyclic aromatic hydrocarbons by gas chromatography–mass spectrometry

“…In general, PCNs and ClPAHs have been analyzed by highresolution gas chromatography (HRGC)-high resolution mass spectrometry (HRMS) and gas chromatography (GC)-mass spectrometry (MS). PCNs have been commonly detected by HRGC-HRMS or GC-MS-MS combined with electron ionization (EI) and separated with a nonpolar fused-silica capillary column such as an Agilent DB-5 column (60 m × 0.25mm inner diameter, 0.25-μm film thickness) [2,[7][8][9]. They have also been analyzed with a GC-MS system equipped with an electron capture negative ion detector and a nonpolar column.…”

Dioxin and Related Compound Detection: Perspectives for Optical Monitoring

“…Even thought Liquid Chromatography coupled to Mass Spectrometry (LC/MS) offers similar advantages, it does not supply a specific interface appropriate for the separation of all the PHAs at the same time [28,31].…”