We developed and evaluated a simple liquid-chromatographic method for urinary pentachlorophenol (PCIP) determination with ultraviolet detection. PCIP and the internal standard (2,3,5,6-tetrachlorophenol, TCP) were extracted with a solid-phase extraction column, and 50 microL of the collected eluate was injected into the chromatograph. The intra-assay and interassay CVs were 6.6% (n = 20) and 7.9% (n = 10), respectively. The analytical recoveries varied from 89% to 96%, with absolute recoveries ranging from 82% to 88%. Thirty urine specimens collected from 30 unexposed individuals were analyzed by the current method, and results were all less than the minimum detection limit, 0.25 mg/L. Results for five specimens from workers who had been exposed to PCIP ranged from 7.0 to 12.4 mg/L. The standard curve was linear to 300 mg/L. This procedure is adaptable to automated analysis, and therefore suitable for monitoring industrial exposure of workers.