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Abuse of mephedrone (4-methylmethcathinone) has emerged among the last few years. Intoxication and fatality associated with mephedrone have been reported in the literature. The present work describes a simple and rapid gas chromatography–mass spectrometry (GC–MS) method for detection and quantification of mephedrone in human blood samples using GC–MS. Blood was deproteinated with acetonitrile and the supernatant was derivatized and extracted in a single step with ethyl chloroformate and ethyl acetate. Methamphetamine-d5 was used as an internal standard (IS). The characteristic ions at  m / z  58, 119 and 130 for mephedrone and  m / z  62, 92 and 134 for methamphetamine-D5 were used for quantification of the analyte. The calibration curve was linear within the concentration range 10–2,000 ng/mL. Intra- and inter-assay precisions (%RSD) were within 10.9–11.9 and 9.2–11.2, respectively. Intra-assay accuracy (%Bias) was between 1.8 and 2.8. The method was successfully applied to detect and quantify mephedrone in real blood samples.

GC–MS Method for Quantification of Mephedrone in Human Blood Sample