title: 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.
abstract: 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 0.6-19.1pgg(-1) and 0.4-8.6pgg(-1), respectively. The PCNs and dl-PCBs levels in these samples ranged from 0.16 to 3.07ngg(-1) dry weight (dw) and from undetectable to 0.07ngg(-1) dw, respectively.
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Fang
authors.initials: F
authors.lastname: Li
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China.
authors.forename: Jing
authors.initials: J
authors.lastname: Jin
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Dongqin
authors.initials: D
authors.lastname: Tan
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Jiazhi
authors.initials: J
authors.lastname: Xu
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China.
authors.lastname: Dhanjai
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China.
authors.forename: Yuwen
authors.initials: Y
authors.lastname: Ni
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China.
authors.forename: Haijun
authors.initials: H
authors.lastname: Zhang
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China. Electronic address: chenjp@dicp.ac.cn.
authors.forename: Jiping
authors.initials: J
authors.lastname: Chen
mesh_terms: D000818:Animals; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D019015:Geologic Sediments / Q000737:chemistry; D009281:Naphthalenes / Q000032:analysis*; D049897:Pectinidae / Q000737:chemistry; D028223:Pinus / Q000737:chemistry; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D009281:Naphthalenes; D011078:Polychlorinated Biphenyls
keywords: Cleanup; Dioxin-like polychlorinated biphenyls; Magnesium oxide; Polychlorinated naphthalenes; Solid-phase extraction