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A simple and highly sensitive voltammetric method was developed for the determination of benazepril (I) and ramipril (II). The compounds were treated with nitrous acid, and the cathodic current produced by the resulting nitroso derivatives was measured. The voltammetric behavior was studied by adopting direct current (DCt), differential pulse (DPP), and alternating current (ACt) polarography. Both compounds produced well-defined, diffusion-controlled cathodic waves over the whole pH range in Britton-Robinson buffers (BRb). At pH 3 and 5, the values of diffusion-current constants (Id), were 5.90 ± 0.40 and 6.66 ± 0.61 for I and II, respectively. The current–concentration plots for I were rectilinear over the range of 1.5–40 and 0.1–30 μg/mL in the DCt and DPP modes, respectively; for II, the range was 2–30 and 0.1–20 μg/mL in the DCt and DPP modes, respectively. The minimum detectabilities (S/N = 2) were 0.015 μg/mL (about 3.25 × 10−8M) and 0.012 μg/mL (about 2.88 × 10−8M) for I and II, respectively, adopting the DPP mode. Results obtained for the proposed method when applied to the determination of both compounds in dosage forms were in good agreement with those obtained using reference methods. Hydrochlorthiazide, which is frequently co-formulated with these drugs, did not interfere with the assay. The method was also applied to the determination of benazepril in spiked human urine and plasma. The percentage recoveries adopting the DPP mode were 96.2 ± 1.21 and 95.7 ± 1.61, respectively.