title: Analysis of selected designer benzodiazepines by ultra high performance liquid chromatography with high-resolution time-of-flight mass spectrometry and the estimation of their partition coefficients by micellar electrokinetic chromatography.
abstract: A new ultra high performance liquid chromatography with electrospray ionization time of flight mass spectrometry method for the selective and sensitive separation, identification, and determination of selected designer benzodiazepines (namely, pyrazolam, phenazepam, etizolam, flubromazepam, diclazepam, deschloroetizolam, bentazepam, nimetazepam, and flubromazolam) in human serum was developed. The separation of the studied designer benzodiazepines was achieved on C18chromatographic column using gradient elution within 6 min without any significant matrix interferences. Liquid-liquid extraction with butyl acetate was applied for serum samples cleanup and preconcentration of studied designer benzodiazepines. The method was validated in terms of linearity, limit of detection, limit of quantification, matrix effects, specificity, precision, accuracy, recovery, and sample stability. The limit of detection values were 0.10-0.15 ng/mL. The method was applied to a spiked serum sample to demonstrate its applicability for systematic toxicology analysis. Furthermore, a capillary chromatographic method with micellar electrokinetic chromatography was used for the estimation of partition coefficients of studied designer benzodiazepines as important parameters to evaluate their pharmacological and toxicological properties.
authors.affiliation: Department of Forensic Medicine and Medical Law, Faculty Hospital, Olomouc, Czech Republic.
authors.forename: Jana
authors.initials: J
authors.lastname: Tomková
authors.affiliation: Department of Analytical Chemistry, Regional Centre of Advanced Technologies and Materials, Faculty of Science, Palacky University in Olomouc, Olomouc, Czech Republic.
authors.forename: Martin
authors.initials: M
authors.lastname: Švidrnoch
authors.affiliation: Department of Analytical Chemistry, Regional Centre of Advanced Technologies and Materials, Faculty of Science, Palacky University in Olomouc, Olomouc, Czech Republic.
authors.forename: Vítězslav
authors.initials: V
authors.lastname: Maier
authors.affiliation: Department of Forensic Medicine and Medical Law, Faculty Hospital, Olomouc, Czech Republic.
authors.forename: Peter
authors.initials: P
authors.lastname: Ondra
mesh_terms: D001569:Benzodiazepines / Q000097:blood*; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D057230:Limit of Detection; D008823:Micelles; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D008823:Micelles; D001569:Benzodiazepines
keywords: benzodiazepines; liquid chromatography; mass spectrometry; micellar electrokinetic chromatography; partition coefficients