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The drug and internal standard were isolated from plasma by extraction with dichloromethane and 2 <jats:sc>M<\/jats:sc> hydrochloric acid. Chromatographic separation was performed on a C<jats:sub>18<\/jats:sub> column with methanol_water (68:32, v\/v) adjusted to pH 3.2 with phosphoric acid as mobile phase. The oxidation potential for detection was established by constructing a voltammogram for diclofenac. The quantification limit for diclofenac in plasma was 5 ng mL<jats:sup>\u22121<\/jats:sup>. Linearity of the method was confirmed in the range 5_2000 ng mL<jats:sup>\u22121<\/jats:sup>, correlation coefficient 0.9998. Within\u2010day relative standard deviations (RSDs) ranged from 0.66 to 14.00% and between\u2010day RSDs from 0.59 to 15.78%. The method was successfully applied for the determination of pharmacokinetic parameters after ingestion of a 50 mg dose of diclofenac. Studies were performed on 18 healthy volunteers of both sexes. 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