A method is described for the simultaneous quantification of cocaine, benzoylecgonine, and cocaethylene in pericardial fluid. Pericardial fluid samples from autopsy casework involving cocaine-related deaths and deaths unrelated to drug abuse were collected. The extraction of cocaine and its metabolites was performed using Bond-Elut Certify columns. Pericardial fluid samples were adjusted to pH 7 and applied to the pre-conditioned cartridges. After the washing steps, compounds were eluted with a mixture of chloroform/isopropanol (80:20) with 2% ammonium hydroxide. The dry extracts were derivatized with pentafluoropropionic anhydride and hexafluoroisopropanol and analyzed by gas chromatography-mass spectrometry using electron impact ionization and selective ion monitoring acquisition. Deuterated internal standards were used. The analytical method developed was linear, sensitive, selective, accurate, and sufficiently precise to be applied routinely in forensic toxicology. In this study, the procedure has been successfully applied to a number of forensic cases involving cocaine intoxication.