A simple, rapid, and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the determination of zinc pyrithione (ZnPT) and pyrithione (PT) in shampoos. The method consisted of a liquid–liquid extraction for sample preparation. The mass spectrometer was operated in multiple reaction monitoring (MRM) mode via the positive electrospray ionization interface. A linear regression (weighted 1/x) was used to fit calibration curves over the concentration range of 50–2000 ng/mL for both ZnPT and PT. Excellent linearity (r2 ≥ 0.9996) was achieved for all. The method was validated and found to be accurate (95.9–108.2% for ZnPT and 94.9–110.4% for PT), precise, and selective. Analytes in shampoos were found to be stable in the autosampler (6 °C for 6 h), in room temperature (for 6 h), and after three freeze–thaw cycles, and recovery of analytes was reproducible (90.8–94.6% for ZnPT and 90.2–96.3% for PT).