An accurate, simple, reproducible and sensitive method for the determination of paracetamol, caffeine and dipyrone was developed and validated. Paracetamol, caffeine and dipyrone were separated using a µ-Bondapack C8 column by isocratic elution with a flow rate of 1.0 ml/min. The mobile phase composition was 0.01 M KH2PO4−-methanol-acetonitrile-isopropyl alcohol (420: 20: 30: 30) (v/v/v/v) and spectrophotometric detection was carried out at 215 nm. The linear range of determination for paracetamol, caffeine and dipyrone were 0.409-400 µg/ml, 0.151-200 µg/ml and 0.233-600 µg/ml, respectively. The method was shown to be linear, reproducible, specific, sensitive and rugged.