A new laboratory experiment is described in which students compare two benchtop separation methods to isolate the three active components of the commercial analgesic Excedrin. In the two-week sequence, aspirin, acetaminophen, and caffeine are separated using either a two-base liquid-liquid extraction or silica column chromatography. Students then evaluate the two separation methods based on percent recoveries and on purity, as determined by thin-layer chromatography. This procedure introduces three important techniques using a single theme. The experiment has been designed to minimize cost of chemicals and hazardous waste generation, while challenging students to critically evaluate the strengths and weaknesses of different purification techniques. (Contains 2 figures.)