జర్నల్ ఆఫ్ క్రోమాటోగ్రఫీ & సెపరేషన్ టెక్నిక్స్
అందరికి ప్రవేశం

నైరూప్య

Simultaneous Quantitative Determination of Synthetic Cathinone Enantiomers in Urine by GC-NCI-MS/MS using Menthylchloroformate as Chiral Derivatization Reagent

Meetani MA*, Alzaabi JA, Hisaindee S, Altabaji MK, Alremeithi R

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 been 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), interday 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.