A reliable and reproducible high performance liquid chromatography method with coulometric detection was developed and validated for the quantitative determination of trace-levels of hydrogen peroxide in crospovidone, a pharmaceutical excipient, and a capsule pharmaceutical product. The method conditions included: a reproducible extraction procedure to provide a concentrated extract, aqueous extraction solvent; a simple HPLC mobile phase (aqueous 50 mM ammonium acetate) compatible with the coulometric detection; a reserve-phase HPLC column that did not collapse under 100% aqueous mobile phase conditions providing sufficient retention and separation of hydrogen peroxide from interferences; and a coulometric detector with a multi-electrode array providing sensitive and selective detection. The method validation results, including those for specificity, linearity, accuracy, precision, and recovery, were acceptable for the determination of trace levels of hydrogen peroxide. The method was shown to be linear over the range of 0.6–4.5 ppm (μg/g) and 6–90 ppm (μg/g) for the pharmaceutical product and crospovidone, respectively. The described method was applied to the determination of trace levels of hydrogen peroxide in different batches of crospovidone and the corresponding pharmaceutical product batches manufactured from these batches of this excipient.