title: Fast separation of selected cathinones and phenylethylamines by supercritical fluid chromatography.
abstract: The chromatographic behaviour of eleven synthetic cathinones and four phenylethylamines under supercritical/subcritical fluid conditions was investigated. Four stationary phases with sub-2μm particles (Waters Acquity UPC(2) BEH silica, BEH 2-ethylpyridine, CSH Fluoro-Phenyl, and HSS C18SB) were evaluated in terms of isomer resolution, chromatographic peak shape, and analysis time. Methanol, water, formic acid, ammonium hydroxide, ammonium acetate, and ammonium formate were mixed with carbon dioxide to test their influence on analyte retention and peak shapes. Methanol and ammonium cations were essential for successful separations. Efficient separations of four isomeric pairs (R>1), and most of the remaining analytes, were achieved in less than 3.3min on BEH and Fluoro-Phenyl columns with gradient of methanolic ammonium hydroxide in CO2. Drugs were detected by positive electrospray ionization-triple quadrupole mass spectrometry in selected reaction monitoring mode. Added detection specificity and faster separation of isomers on the BEH column using a steep gradient and high flow rate reduced analysis time of the mixture of 15 drugs to 1.6min.
authors.affiliation: Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacký University in Olomouc, 17. listopadu 12, 771 46 Olomouc, Czech Republic.
authors.forename: Volodymyr
authors.initials: V
authors.lastname: Pauk
authors.affiliation: Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacký University in Olomouc, 17. listopadu 12, 771 46 Olomouc, Czech Republic.
authors.forename: Veronika
authors.initials: V
authors.lastname: Žihlová
authors.affiliation: Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacký University in Olomouc, 17. listopadu 12, 771 46 Olomouc, Czech Republic.
authors.forename: Lucie
authors.initials: L
authors.lastname: Borovcová
authors.affiliation: Institute of Microbiology, v.v.i., Videnska 1083, 142 20 Prague 4, Czech Republic.
authors.forename: Vladimír
authors.initials: V
authors.lastname: Havlíček
authors.affiliation: Department of Chemistry and Biochemistry, The University of Texas at Arlington, Arlington, TX 76019, USA.
authors.forename: Kevin
authors.initials: K
authors.lastname: Schug
authors.affiliation: Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacký University in Olomouc, 17. listopadu 12, 771 46 Olomouc, Czech Republic. Electronic address: Karel.Lemr@upol.cz.
authors.forename: Karel
authors.initials: K
authors.lastname: Lemr
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D025924:Chromatography, Supercritical Fluid; D000432:Methanol / Q000737:chemistry; D010627:Phenethylamines / Q000032:analysis*
chemical_list: D000470:Alkaloids; D010627:Phenethylamines; C023665:cathinone; D000432:Methanol
keywords: Cathinones; Electrospray ionization mass spectrometry; New designer drugs; Phenylethylamines; Supercritical fluid chromatography