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A method is proposed for the determination of the cytotoxic antineoplastic drug cisplatin in blood plasma by reversed-phase high-performance liquid chromatography with mass spectrometry detection. The conditions of the formation of a cisplatin derivative with sodium diethyl dithiocarbamate and its isolation from the matrix using solid-phase extraction on a hydrophilic lipophilic adsorbent Oasis HLB are optimized. The limit of the quantitative determination of cisplatin was 10 ng/mL. The method is validated in accordance to the Food and Drug Administration (FDA) requires and was appllied to the pharmacokinetical study on the isolated lung perfusion by cisplatin.