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Fast miniaturised sample preparation for the screening and comprehensive two‐dimensional gas chromatographic determination of polychlorinated biphenyls in sludge
Author(s) -
Kristenson E. Maria,
Neidig Harmen C.,
Vreuls René J. J.,
Brinkman Udo A. Th.
Publication year - 2005
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301733
Subject(s) - chromatography , sample preparation , gas chromatography , chemistry , environmental chemistry , environmental science
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.