Determination of pentachlorophenol in wood samples using liquid chromatography with UV absorbance, amperometric and...

The potential of reversed-phase liquid chromatography (RPLC) with UV and amperometric detection (AD), and of normal-phase liquid chromatography (NPLC) with UV and electron-capture detection (ECD) for the determination of pentachlorophenol (PCP) in wood samples has been studied. When PCP concentrations of at least 1-5 ppm have to be determined, RPLC-UV and RPLC-AD on C18-modified silica are useful techniques, provided a two- or three-step sample-preparation step is used. NPLC-UV on bare silica columns does not offer any advantage over RPLC-UV. NPLC-ECD on bare silica and with an acidified toluene-hexane mixture as eluent offers good selectivity and sensitivity, as well as satisfactory linearity and reproducibility for the determination of PCP in wood samples down to low ppb levels. Use of the two-step clean-up procedure is sufficient, and even a single-step procedure has been utilized. In the latter case, analysis times are longer because of the presence of late-eluting ECD-active interferences. The two-step clean-up procedure generally used involves a liquid-liquid extraction with dichloromethane, and solid-liquid sorption using a Sep Pak C18 cartridge. PCP recovery over the 0.2-10 ppm range is 75-100%. Several wood samples containing 1-50 ppm of PCP have successfully been analyzed, and the good potential of NPLC-ECD for trace-level determination of PCP has been demonstrated.