A simple, sensitive and selective square-wave adsorptive stripping voltammetric method has been developed and validated for the determination of nifedipine (NIF) in plasma. The assay was performed after single extraction of NIF from alkalinised plasma into organic phase. The adsorption behaviour of NIF on a hanging mercury drop electrode (HMDE) was explored by square-wave and cyclic voltammetry. The drug was accumulated at HMDE and a well-defined peak was obtained at - 730 mV versus Ag/AgCl in borate buffer of pH 9.0 including 0.01 M KCI. The linear concentration range was 2.89 x 10(-9) M-3.61 X 10(-7) M (1.00-125.01 ng ml(-1)) when using 30 s accumulation time at - 300 mV. Limit of detection and limit of quantification were 1.21 x 10(-9) M (0.42 ng ml(-1)) and 2.89 x 10(-9) M (1.00 ng ml(-1)) respectively. The intra-day relative standard deviation (RSD) ranged from 1.93 to 4.12% at three concentrations and the inter-day RSDs varied from 2.53 to 6.68%. The method was applied, to the plasma of pregnant women suffering from pregnancy induced hypertension, for the determination of NIF. The percentage recoveries varied from 96.26 to 99.49%. It has been shown that NIF could be determined in the presence of its main metabolite (dehydronifedipine) by the developed method. (C) 2002 Elsevier Science B.V. All rights reserved.