Fluconazole concentrations in biological fluids were determined by high-performance gas chromatography. A simple extraction procedure with chloroform, under basic conditions and after the addition of UK-47,265 as the internal standard and with no evaporation stage, was carried out prior to analysis. A solid injector and a 15-m capillary column, coated with a nonpolar phase and connected to a nitrogen-selective detector that afforded an excellent selectivity and sensitivity, constituted the gas chromatographic system. The duration of each analysis was less than 4 min and the minimum detectable serum concentration was 50 ng/mL. In five patients undergoing chronic peritoneal dialysis, the mean serum concentrations +/- SD at 1, 6, and 48 h after the intraperitoneal administration of a single dose of fluconazole were, respectively, 325 +/- 75, 928 +/- 159, and 607 +/- 80 ng/mL.