AbstractA rapid, sensitive, and reliable method for the determination of nifedipine in human plasma is described. Using a single‐step solvent extraction and capillary gas chromatography combined with electron capture detection, an assay sensitivity of 2 ng/ml is achieved routinely using 0.5 ml of plasma. Intact nifedipine is quantitated and separated from its nitroso‐ and nitropyridine‐derivatives. The suitability of the assay for pharmacokinetic studies is illustrated.