Development and validation of a new analytical method for enantioseparation and quantitation of synthetic cathinones is reported using a chiral derivatization agent (CDA) and GC-MS triple quadrupole mass spectrometry with negative chemical ionization (NCI) mode. Indirect separation of ten synthetic cathinone compounds has be achieved using a commercially available optically pure CDA called (1R)-(-)-menthylchloroformate (MCF). MCF was capable of converting synthetic cathinone enantiomers into diastereoisomers, which were later separated with good resolution on an ultra-inert 60 m achiral stationary phase column. An internal standard (IS), 3-methylmethcathinone (3-MMC) was used for quantitation of synthetic cathinone diastereoisomers. Method validation in terms of calibration curve linearity, sensitivity in terms of limits of detections (LODs), limits of quantitation (LOQs), inter-day and intra-day reproducibility, and recoveries has been obtained for the ten synthetic cathinone compounds that were analyzed simultaneously as a mixture after being spiked in urine. It was found that LOD’s and LOQ’s for the ten synthetic cathinones mixture in urine were in the ranges of 0.004-3.678 ppm and 0.012-11.14 ppm respectively. The results of four synthetic cathinones (Buphedrone, 3-MethylBP,3,4-DMEC, and Butylone) derivatized with MCF were compared with the same compounds derivatized with N-trifluoroacetyl-L-prolyl chloride (L-TPC). It was found that the later was more sensitive in terms of LOD and LOQ than the former method.

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