The phencyclidine (PCP) analogue 3-HO-PCP, a potent dissociative new psychoactive substance, was detected in a law enforcement seizure and forensic samples in Denmark. Its toxicokinetic properties were investigated for the first time. The unbound fraction in plasma was 0.72 ± 0.09. Four in vitro metabolites were identified after incubation with human hepatocytes; in vivo, the O-sulphate-conjugated metabolite was not detected, and the N-dealkylated-COOH metabolite was the main metabolite in deconjugated urine. In blood and brain, 3-HO-PCP and its O-glucuronidated metabolite were the primary analytical targets. Drug levels in blood were 0.013 mg/kg in a living subject and 0.095 mg/kg in a deceased subject. Post-mortem brain concentration was 0.16 mg/kg, 1.5-fold higher than in post-mortem blood.