新型持久性有机污染物分析方法研究进展

Polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs), perfluorooctanoic acid (PFOA), perfluorooctyl sulfonates (PFOS), chlordecone and polybrominated dibenzo-p-dioxin and dibenzofurans (PBDD/Fs), as the new listed POPs in Stockholm Convention and emerging POPs, were increasingly concerned by environmental scientists. The research work about the residue’s characteristic, source analysis, trends evolution, transport, bioaccumulation, and toxic effects of these emerging chemicals depended on the development of the analytical methods. Analytical procedures of PBDEs and PBBs were similar to those of organochlorine pesticides (OCPs) and poly chlorinated biphenyls (PCBs), due to their similar physical and chemicalcharacteristics with “Dirty Dozen”. Many extraction methods, such as Soxhlet extraction, automatic Soxhlet extraction, supersonic extraction, microwave assisted extraction, pressurized fluid extraction, were applied for water, sediment, soil and particulate matter. Common clean-up steps were sulfuric acid silica gel cartridge, multiple layer chromatography column and GPC. Although HRGC/HRMS and GC/MS/MS were effective for environmental background samples, GC/MS-EI and GC/MS-NCI were most popular for determinations of the PBDEs and PBBs indicators or markers. HPLC/MS/MS with solid phase extraction was developed for the perfluorinated alkyl acids, sulfonates and their salts. HLB solid phase column was efficient for PFOA/PFOSs recoveries from water samples, as the weak anion exchange column could raise the recoveries of perfluorinated alkyl acids and sulfonates with the carbon chain ranging from 4 to 14. Acetone was necessary in the extraction because of the polarity of clordecone. The GC injector and capillary column needed cleaning carefully when clordecone was analyzed by GC/ECD and GC/MS, otherwise the strong tailing of chromatographic peak would make the exact qualitative and quantitative impossible. The analysis procedures for polybrominateddibenzo-p-dioxin and dibenzofurans (PBDD/Fs) were similar to those of PCDD/Fs. Florisil or active carbon-impregnated silica gel column were packed to separate PBDEs and PBDD/Fs. The instrumental conditions were optimized to prevent from the thermal degradation of higher brominated compounds. The application of the method was also depended on the improvement of PBDD/Fs reference materials.