Method development of combining pressurized liquid extraction and off-line HPLC fractionation with a porous graphite carbon column for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in environmental samples

摘要

A method was developed for analysis of PCDD/Fs in fly ash and soil samples by using the combination of pressurized liquid extraction (PLE) and off-line HPLC fractionation with a porous graphite carbon (PGC) column, followed by analysis using HRGC/HRMS. The samples were automatically extracted by PLE. A multi-layer silica column was used for the preliminary cleanup. Then off-line fractionation was applied for the separation of PCDD/Fs and the collected PCDD/Fs fraction was analyzed by HRGC/HRMS. The use of solvent back-flushing at 70℃ successfully solved the carry-over problem of PGC column. The procedure of single extraction and cleanup provided advantages of high automation and significant reduction of solvent and time compared to conventional methods. The method was validated by certified materials of fly ash and industrial sandy soil, and applied for the analysis of fly ash samples collected from three two-ton medical waste incinerators in Beijing and one farm soil sample collected in the vicinity of the incinerators.