MARDONES, C.; VON BAER, D.; HIDALGO, A.; CONTRERAS, A.; SEPÚLVEDA C.
Journal of Separation Science 31(2008) 1124-1129.
DOI: 10.1002/jssc.200700403
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 GC/MS 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 Na2CO3, and injected into the CE equipment. The optimal option for GC/MS was extraction with Na2CO3 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.