A high performance liquid chromatographic method for the simultaneous determination of metronidazole and diloxanide furoate in single and combined dosage form has been developed. Each drug acted as internal standard for the other. Both of the drugs eluted from the cyclobond column (β-cyclodextrin stationary phase) without retardation effects, using methanol-0.05 M NaH2PO4(pH 7) in ratio 35:65, flow rate 1 ml min−1and detection at 254 nm. Metronidazole and diloxanide furoate gave rectilinear calibration graphs in the ranges 1–10 μg and 1–5 μg respectively.