TY - JOUR
T1 - Fast miniaturised sample preparation for the screening and comprehensive two-dimensional gas chromatographic determination of polychlorinated biphenyls in sludge
AU - Kristenson, E.M.
AU - Neidig, H.C.
AU - Vreuls, R.J.J.
AU - Brinkman, U.A.T.
PY - 2005
Y1 - 2005
N2 - Polychlorinated biphenyls (PCBs) in sludge are usually extracted by a technique such as Soxhlet with subsequent fractionation prior to long GC runs using GC-ECD or GC-HRMS. In this study, the extraction of selected chlorinated biphenyls (CBs) from a spiked sludge sample by three rapid techniques, i.e. ultrasonic (USE), pressurised-liquid (PLE), and microwave-assisted (MAE) extraction using a domestic microwave, was studied, with subsequent direct GC-ECD, GC-MS, or GC × GC-μECD analysis of the extracts. The main goal was to select an appropriate, and miniaturised, extraction method after only a brief optimisation and demonstrate the power of GC × GC analysis of dirty extracts. For PLE similar CB recoveries were found when extracting with either n-hexane or n-hexane/acetone (1/1). For USE and MAE, n-hexane/acetone (1/1) was the preferred extraction solvent. USE gave the best recoveries (80-95%; except 130% for CB 105). The only clean-up needed prior to GC-MS or GC × GC-μECD analysis was the removal of sulphur-containing compounds. GC-ECD was not suitable for these dirty extracts. The lowest LODs for the CBs (20 fg or 0.1 ng/g sludge) were found when combining USE and GC × GC-μECD, because of the powerful extraction, high separation power and excellent detectability provided by this technique. © 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
AB - Polychlorinated biphenyls (PCBs) in sludge are usually extracted by a technique such as Soxhlet with subsequent fractionation prior to long GC runs using GC-ECD or GC-HRMS. In this study, the extraction of selected chlorinated biphenyls (CBs) from a spiked sludge sample by three rapid techniques, i.e. ultrasonic (USE), pressurised-liquid (PLE), and microwave-assisted (MAE) extraction using a domestic microwave, was studied, with subsequent direct GC-ECD, GC-MS, or GC × GC-μECD analysis of the extracts. The main goal was to select an appropriate, and miniaturised, extraction method after only a brief optimisation and demonstrate the power of GC × GC analysis of dirty extracts. For PLE similar CB recoveries were found when extracting with either n-hexane or n-hexane/acetone (1/1). For USE and MAE, n-hexane/acetone (1/1) was the preferred extraction solvent. USE gave the best recoveries (80-95%; except 130% for CB 105). The only clean-up needed prior to GC-MS or GC × GC-μECD analysis was the removal of sulphur-containing compounds. GC-ECD was not suitable for these dirty extracts. The lowest LODs for the CBs (20 fg or 0.1 ng/g sludge) were found when combining USE and GC × GC-μECD, because of the powerful extraction, high separation power and excellent detectability provided by this technique. © 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
U2 - 10.1002/jssc.200301733
DO - 10.1002/jssc.200301733
M3 - Article
SN - 1615-9306
VL - 28
SP - 1121
EP - 1128
JO - Journal of Separation Science
JF - Journal of Separation Science
IS - 11
ER -