Abstract

An ultrasonic bar-assisted extraction and CE separation procedure for the determination of pentachlorophenol (PCP) and 2,4,6-tribromophenol (TBP) residues in sawdust was developed and applied. For this purpose, micellar electrokinetic capillary chromatography (MEKC) was used and compared with a GCIMS methodology. This methodology allowed the quantification of PCP and TBP in a concentration range of 2.5 - 12.0 mg/ kg for TBP and 2.8 - 12.0 mg/kg for PCP. Different sample treatment processes were evaluated in order to extract these compounds from sawdust. Better results were obtained when the residues were extracted with ultrasound-assisted hexane, filtered, evaporated, dissolved in Na 2CO 3, and injected into the CE equipment. The optimal option for GC/ MS was extraction with Na 2CO 3 followed by a derivation using acetic anhydride and liquid-liquid extraction with hexane. This method allowed the quantification of TBP and PCP in sawdust in a concentration range of 0.19-12.00 mg/kg and 0.14-12.00 mg/kg, respectively. The CE method was compared with the GC/MS as reference method. The results were shown to be statistically similar by both methods for PCP as well as for TBP. © 2008 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.