High performance solid-phase extraction cleanup method coupled with gas chromatography-triple quadrupole mass spectrometry for analysis of polychlorinated naphthalenes and dioxin-like polychlorinated biphenyls in complex samples

A solid-phase extraction (SPE) cleanup method was developed to purify the sample extracts for the analysis of polychlorinated naphthalenes (PCNs) and dioxin-like polychlorinated biphenyls (dl-PCBs). Monodisperse magnesium oxide (MgO) microspheres and basic alumina were used as SPE adsorbents. Important parameters of the SPE procedure were optimized, including the amount of basic alumina and the type and volume of the washing and elution solvents. The optimized SPE cleanup method exhibited excellent purification performance for the removal of organochlorinated compounds, lipid compounds, sulfur, and pigments. Additionally, it was found that the retention activities of congeners differed with the number and position of the chlorine substituents in PCNs. In this study, an analytical method based on a combination of accelerated solvent extraction (ASE) coupled with SPE cleanup and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) is proposed for the analysis of PCNs and dl-PCBs in complex samples (sediment, pine needle, and scallop samples). The analytical method demonstrates good linearity, acceptable recovery (63-148%) and precision (relative standard deviations less than 26%). The limits of detection (LODs) of PCN and dl-PCB congeners were in the range of 0.6-19.1 pg g−1 and 0.4-8.6 pg g−1, respectively. The PCNs and dl-PCBs levels in these samples ranged from 0.16 to 3.07 ng g−1 dry weight (dw) and from undetectable to 0.07 ng g−1 dw, respectively.