Clidinium bromide is a quaternary ammonium anticholinergic agent with peripheral effects. It is commercially available in combination with chlordiazepoxide. There is no official compendial method available for the analysis of both compounds concurrently. Conventional methods for determining both compounds involve extensive extraction and thus are time-consuming, and lack precision. The analytical scheme described in this paper provides a fast and reliable reverse-phase HPLC for chlordiazepoxide and clidinium bromide in pharmaceutical combinations. The mobile phase was 0.04 M ammonium acetate in 70% acetonitrile solution with 1% dimethylformamide (pH 6). The column was microPak MCH-10 (300.0 mm × 4.0 mm), UV detection at 254 nm and benzophenone was used as internal standard. The method was confirmed for linearity, recovery, specificity, accuracy, and applicability.