Methodological Refinements in the Determination of 146 Polychlorinated Biphenyls, Including Non-Ortho- and Mono-Ortho-Substituted PCBs, and 26 Organochlorine Pesticides as Demonstrated in Heron Eggs

Abstract

A method for the determination of 146 polychlorinated biphenyls (PCBs), including four non-ortho- and eight mono-ortho-substituted congeners, and 26 chlorinated pesticides is described. The method consists of ultrasonic extraction, Florisil cleanup, HPLC fractionation over porous graphitic carbon (PGC), and final determination with GC/ECD, GC/MS, or both. Two PCB congeners (PCB 30 and PCB 161) and two polybromobiphenyls (2,4',5-tribromobiphenyl and 3,3',4,4'-tetrabromobiphenyl) were used as surrogate standards to evaluate the analytical efficiency. Four PCB congeners, PCB 14 and PCB 159 for the first fraction, PCB 61 for the second fraction, and PCB 204 for the third fraction, were used as internal standards to monitor the GC performance. The retention behavior of PCBs and pesticides on the PGC column are discussed. The method was found to be reproducible, effective, and reliable under the operational conditions proposed and was applied successfully to the analysis of individual PCBs and chlorinated pesticides in black-crowned night heron (Nycticorax nycticorax) egg samples.

Analytical methods for PCBs and organochlorine pesticides in environmental monitoring and surveillance: a critical appraisal

“…The use of GC–MS allows for the application of isotope-dilution techniques and these have increasingly come into routine use for PCB/OCP analysis in environmental samples due to the sensitivities of the latest generation of quadrupole and ion-trap MS systems [111, 112]. A wide range of PCBs and OCPs are available as 13 C-labeled compounds from several chemical supply companies, which, when added at the extraction step, increase precision and reproducibility for the native analytes.…”

Effect-Directed Analysis of Complex Environmental Contamination

“…For the separation of electron-deficient aromatic compounds, particularly PCBs, PCDD/Fs, and PCNs, PYE phases are frequently used in EDA and conventional chemical analysis of sediments and other environmental samples [134,153,[170][171][172][173][174]. Alternative stationary phases with similar elution characteristics include porous graphitized carbon [154, 175,176], C 60 /C 70 fullerenes bound to polystyrene divinylbenzene [177], and C18 dispersed PX-21 activated carbon [178]. 6).…”

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

“…In recent years, off-line fractionation using HPLC has received more and more attention for PCDD/Fs analysis because of its higher reproducibility, lower solvent consumption and higher potential of automation. As a promising stationary phase used in HPLC column, porous graphite carbon (PGC) has been proven effective for separating PCBs from matrix-related interferences because of its unique homogeneous nature of active sites [15][16][17]. Compared to the conventional cleanup sorbents used for PCDD/Fs analysis, PGC can be recycled by backflushing and is more suitable for automation.…”

“…PLE or off-line fractionation using HPLC has been separately reported in previous literatures for the automation of PCDD/Fs analysis [6,7,12,[15][16][17]. The aim of this study was to develop a more automatic and robust PCDD/Fs analytical method by combining these two techniques.…”