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A sensitive and selective method for the determination of cotinine in plasma and urine is presented. Quantitation is effected by capillary gas chromatography-mass spectrometry after liquid--liquid extraction of 0.25-1 ml of biological specimens with a trideuterated cotinine internal standard. The procedure is linear and has acceptable precision over the range of concentrations encountered in pharmacokinetic studies of nicotine or cotinine. The suitability of the assay is shown by a number of plasma concentration--time curves after a single oral or intravenous administration of cotinine to a human volunteer and after multiple-dose intravenous administration of nicotine.
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