TY - JOUR
T1 - Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements
AU - Strano-Rossi, Sabina
AU - Odoardi, Sara
AU - Castrignanò, Erika
AU - Serpelloni, Giovanni
AU - Chiarotti, Marcello
N1 - Funding Information:
This work was carried out in the framework of the project “Smart Stop” – Control on the sites selling products dangerous for the public health, financed by the Antidrug Policies Department, Presidency of Italian Council of Ministers .
Publisher Copyright:
© 2014 Elsevier B.V.
PY - 2015/3/5
Y1 - 2015/3/5
N2 - 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 25ngg-1 and limits of quantification (LOQ) were 50ngg-1 for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000ng 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.
AB - 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 25ngg-1 and limits of quantification (LOQ) were 50ngg-1 for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000ng 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.
KW - Anorectics
KW - LC-HRMS
KW - Nutritional supplements
KW - PdE5Is
KW - Stimulants
UR - http://www.scopus.com/inward/record.url?scp=84923320201&partnerID=8YFLogxK
U2 - 10.1016/j.jpba.2014.06.011
DO - 10.1016/j.jpba.2014.06.011
M3 - Article
C2 - 24996684
AN - SCOPUS:84923320201
SN - 0731-7085
VL - 106
SP - 144
EP - 152
JO - Journal of Pharmaceutical and Biomedical Analysis
JF - Journal of Pharmaceutical and Biomedical Analysis
ER -