Simultaneous determination of 12 illicit drugs in whole blood and urine by solid phase extraction and UPLC–MS/MS

Abstract A rapid and sensitive method based on solid phase extraction and ultra performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC–ESI-MS/MS) for the simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylene-dioxymethamphetamine, N-methyl-1-(3,4-methyl-enedioxyphenyl)-2-butanamine, 3,4-methylenedioxyethylamphetamine, p-methoxymethamphetamine, ephedrine, N-methylephedrine, cathinone, methcathinone, and ketamine in whole blood and urine was developed and validated. Following solid phase extraction, the analytes were separated on ACQUITY UPLC BEH Phenyl column (100 mm × 2.1 mm, 1.7 μm) under gradient elution using a mobile phase containing of acetonitrile and 0.3% formic acid in water at a flow rate of 0.4 mL min −1 and analyzed by a triplequadrupole mass spectrometer in the multiple reaction monitoring (MRM) mode. The proposed method was linear for each analyte with correlation coefficients over 0.99. Recovery validation studies showed accuracy bias below 4.4%. Acceptable precision was also obtained with a relative standard deviation below 8.9%. The sensitivity of the assay was found to be adequate for the quantitation of the illicit drugs in whole blood and urine sample and was higher than reported methods. The present method was proved to be reliable and robust for drug screening in forensic toxicological analysis.