This laboratory experiment introduces upper-division undergraduate analytical chemistry students to liquid chromatography-tandem mass spectrometry (LC-MS/MS) in a forensic application: the analysis of cocaine and metabolites of cocaine in simulated serum ostensibly from drug overdose victims. For this investigation, students developed the analytical methods. First, the students determined the multiple reaction monitoring (MRM) transitions and optimized collision energy. The MS methods developed were then added to an LC method for LC-MS/MS quantitation with a 2.5 min run time. Students successfully quantified the drugs and metabolites, and they were able to identify which samples indicated cocaine use and overdose.