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This article presents a report on the development and validation of two multi-component quantitative methods using liquid chromatography tandem mass spectrometry for the analysis of benzoylecgonine and ecgonine methyl ester in plasma and urine, as well as cocaine, benzoylecgonine and ecgonine methyl ester in hair, using isotope-labeled analogs as internal standards. Both plasma and hair analyses were performed by solid-phase extraction with LC-MS/MS analysis. Mass spectral conditions were optimized for MS/MS analyses of the cocaine, benzoylecgonine and ecgonine methyl ester drugs with electrospray ionization. The limits of quantitation (LOQ) for cocaine, benzoylecgonine, and ecgonine methyl ester were 5 ng/mL in plasma and 10 ng/mg in hair (10 mg hair sample). The LOQ for cocaine in urine was 10 ng/mL. The method was validated according to guidelines of the U.S. Food and Drug Administration. The recovery of analytical
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