Quantification of nitric oxide in vivo is difficult because of its short half-life. Instead the oxidised products, nitrite and nitrate, are commonly used as indices of nitric oxide generation. We describe here a simple method for the measurement of nitrite and nitrate in plasma using high performance capillary electrophoresis. Plasma standard curves gave regression coefficients of 0.98 for nitrite and 0.99 for nitrate with an intra-assay coefficient of variance of 4.6% for 50 microM nitrite (n = 10) and 1.2% for 50 microM nitrate (n = 10). The assay allows measurement of nitrite and nitrate in a single analysis requiring minimal sample preparation, and with the sensitivity to detect both basal and physiological changes in plasma nitrite and nitrate.