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Abstract-A method has been developed for quantification of phencyclidine [I-( 1 -phenylcyclohexyl)piperidine] in body fluids using gas chromatography chemical ionization mass spectrometry with selected ion recording. Pentadeuterated phencyclidine was synthesized and used as the internal standard. In developing the method it was discovered that phencyclidine thermally fragments to I-phenylcyclohexene at elevated temperatures. The sensitivity and specificity of the method permits determination of 1 ng of phencyclidine in 1 ml of body fluid. The concentrations of the drug in blood samples from five individuals, who ingested unknown quantities of phencyclidine, were found t o range from 50 ng/ml to 2.7 pg/ml. Following intravenous administration of I mg of phencyclidine hydrochloride to a 12.5 kg dog, the blood concentration of the drug peaked at 17.6 ng/ml and exhibited a half-life of approximately one hour. Two metabolites of phencyclidine were detected in human and dog urine after enzymatic hydrolysis. The metabolites were tentatively identified as 4-phenyl-4-piperidinocyclohexanol and 1 -( l-phenylcyclohexyl)-4-hydroxy-piperidine by electron impact and chemical ionization mass spectral analysis of the metabolites and their trimethylsilyl derivatives. Structural confirmation was achieved by synthesis of the metabolites. A third metabolite was found in urine from rhesus monkeys and was tentatively identified as 1 -(I -phenyl-4-hydroxycyclohexyl)-4-hydroxypiperidine.