title: Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements.
abstract: The paper describes a liquid chromatography/high resolution mass spectrometry LC/HRMS method for the simultaneous identification and quantification of stimulants (ephedrines, caffeine, anorectic drugs such as phentermine, phendimetrazine, phenmetrazine, fenfluramine, benfluorex, mephentermine, fencanfamine, sibutramine) and PDE5I (sildenafil, vardenafil and tadalafil) in food supplements using a benchtop Orbitrap mass spectrometer. The mass detector, with a nominal resolving power of 100,000 (FWHM at m/z 200), operated in full scan mode in ESI positive ionization mode. Analytes were identified by retention times, accurate masses and correspondence of experimental and calculated isotopic patterns. The limits of detection (LOD) obtained varied from 1 to 25 ng g(-1) and limits of quantification (LOQ) were 50 ng g(-1) for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000 ng g(-1), giving correlation coefficients>0.99. Accuracy (intended as %E) and repeatability (% CV) were always lower than 15%. The method was applied to the analysis of 36 dietary supplements, revealing the presence of ephedrine and/or pseudoephedrine in four of them, caffeine in eight of them and sildenafil in four of them. In one case, ephedrine was not reported on the label of the dietary supplement, as well as for caffeine in other two cases. A further confirmation of the analytes identity in positive samples was obtained through in-source fragmentation and comparison of the obtained fragments and their relative abundances with those from certified standards. As the acquisition mode is full scan, it would be also possible to re-process a previously acquired datafile for the investigation of untargeted analytes.
authors.affiliation: Institute of Public Health, Forensic Toxicology Laboratory, Università Cattolica del S. Cuore, Rome, Italy. Electronic address: Sabina.stranorossi@gmail.com.
authors.forename: Sabina
authors.initials: S
authors.lastname: Strano-Rossi
authors.affiliation: Institute of Public Health, Forensic Toxicology Laboratory, Università Cattolica del S. Cuore, Rome, Italy.
authors.forename: Sara
authors.initials: S
authors.lastname: Odoardi
authors.affiliation: Institute of Public Health, Forensic Toxicology Laboratory, Università Cattolica del S. Cuore, Rome, Italy.
authors.forename: Erika
authors.initials: E
authors.lastname: Castrignanò
authors.affiliation: Antidrug Policies Department, Presidency of Council of Ministers, Rome, Italy.
authors.forename: Giovanni
authors.initials: G
authors.lastname: Serpelloni
authors.affiliation: Institute of Public Health, Forensic Toxicology Laboratory, Università Cattolica del S. Cuore, Rome, Italy.
authors.forename: Marcello
authors.initials: M
authors.lastname: Chiarotti
mesh_terms: D001067:Appetite Depressants / Q000032:analysis; D000697:Central Nervous System Stimulants / Q000032:analysis; D002853:Chromatography, Liquid / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D004348:Drug Labeling; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D058986:Phosphodiesterase 5 Inhibitors / Q000032:analysis; D015203:Reproducibility of Results
chemical_list: D001067:Appetite Depressants; D000697:Central Nervous System Stimulants; D058986:Phosphodiesterase 5 Inhibitors
keywords: Anorectics; LC–HRMS; Nutritional supplements; PdE5Is; Stimulants