Method development for the analysis of polybrominated diphenyl ethers, polychlorinated biphenyls, polychlorinated dibenzo-p-dioxins and dibenzo-furans in single extract of sediment samples

Abstract

A comprehensive method was developed for quantitative analysis of polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins and dibenzo-furans (PCDD/Fs) in one single extract of environmental samples. The sample preparation procedure included two fractionation steps using silver nitrate silica chromatography to separate PBDEs from PCBs and PCDD/Fs and florisil column to separate PCBs from PCDD/Fs. Acidic silica, acidic alumina and gel permeation chromatography (GPC, for PCBs) or activated carbon column (for PCDD/Fs) were used for further clean-up. The sample extracts were analyzed by using high-resolution gas chromatography/highresolution mass spectrometry. The entire method was validated from the analysis of mixed standards of PBDEs, PCBs and PCDD/Fs (n = 3); the analysis of certified reference biota (WMF-01). The method was applied for the analysis of 10 sediment samples collected from Haihe River and Dagu Drainage River in Tianjin City. No significant PBDEs pollution was found in the areas.

Pulsed large volume injection gas chromatography coupled with electron-capture negative ionization quadrupole mass spectrometry for simultaneous determination of typical halogenated persistent organic pollutants

“…However, GC/MS is preferred now because absolute chromatographic separation for the individual analyte was difficult even if multidimensional GC was employed [10]. Several GC/MS methods have been established based on high-resolution magnetic-sector MS (HR-MS) [11], tandem MS (MS/MS) using an ion trap detector [12][13][14], or triple quadrupole analyzer [15] and time-of-flight MS (TOF-MS) [16], as well as lowresolution quadrupole MS (qMS) [17]. Obviously, HR-MS is the most powerful tool offering high selectivity with satisfactory sensitivity by virtue of its high ultimate resolving power and accurate mass measurement; nevertheless, nowadays only a few laboratories can afford this instrument.…”