Liquid chromatographic determination of pentachlorophenol in serum, using pre-column phase-transfer catalysed dansylation and post-column photolysis with fluorescence detection

Abstract

Dansylation of pentachlorophenol was carried out after solid-phase extraction of acidified human serum and desorption with dichloromethane, in a dichloromethane-water two-phase system using tetrabutyl-ammonium bromide as the phase-transfer catalyst. Derivatisation was complete within 2 min at room temperature. After evaporation of an aliquot of the organic phase, the residue was dissolved in methanol and injected into a reversed-phase chromatographic system, equipped with a post-column photochemical reactor. In the reactor, dansylated pentachlorophenol is converted into highly fluorescent products. The recovery of the analyte from serum was 85 ± 4%. Calibration graphs for horse and human serum were linear over two decades, with correlation coefficients ranging from 0.996 to 0.999. The detection limit of pentachlorophenol in horse and human serum was 400 pg ml^–1. The reproducibility of the total procedure for a human serum sample containing 4 ng ml^–1 was 4.5%.