title: Determination of flibanserin and tadalafil in supplements for women sexual desire enhancement using high-performance liquid chromatography with tandem mass spectrometer, diode array detector and charged aerosol detector.
abstract: The new compound - flibanserin - begun to appear as a synthetic adulterant in counterfeit herbal supplements used to stimulate women sexual drive. It was detected in two samples submitted to the Polish National Medicines Institute for analysis. The second sample contained also tadalafil. This study presents the LC method development which enables the determination of flibanserin and tadalafil. It employs three different detectors charged aerosol detector (CAD), diode array detector (DAD) and mass spectrometer (MS). The conditions of the elaborated method were optimized to obtain the highest sensitivity and the best resolution, especially the separation of icariin - the natural compound observed often in supplements for sexual disorders. The validation of the method proved good linearity, good accuracy and precision of the measurements recorded by all three detectors. Additionally, for CAD data, an alternative calculation method using a unified calibration function was presented and evaluated. It seems that this is the way to overcome the problem of non-availability of the reference standard of a target compound. Flibanserin content was quantified using the data of other reference standard (tadalafil). The inaccuracy of proposed indirect determination was found to be ±3%. A statistical evaluation proved that the results obtained with all detection modes and the results calculated using a unified calibration were not significantly different (p>0.05).
authors: Pharmaceutical Chemistry Department, National Medicines Institute, 30/34 Chelmska Street, 00-725 Warsaw, Poland; Department of Bioanalysis and Drug Analysis, Medical University of Warsaw, 1 Banacha Street, 02-097 Warsaw, Poland. Electronic address: m.poplawska@nil.gov.pl.
authors: Magdalena
authors: M
authors: Poplawska
authors: Pharmaceutical Chemistry Department, National Medicines Institute, 30/34 Chelmska Street, 00-725 Warsaw, Poland.
authors: Agata
authors: A
authors: Blazewicz
authors: Department of Bioanalysis and Drug Analysis, Medical University of Warsaw, 1 Banacha Street, 02-097 Warsaw, Poland.
authors: Paulina
authors: P
authors: Zolek
authors: Pharmaceutical Chemistry Department, National Medicines Institute, 30/34 Chelmska Street, 00-725 Warsaw, Poland; Department of Bioanalysis and Drug Analysis, Medical University of Warsaw, 1 Banacha Street, 02-097 Warsaw, Poland.
authors: Zbigniew
authors: Z
authors: Fijalek
mesh_terms: D000336:Aerosols / Q000737:chemistry; D001562:Benzimidazoles / Q000737:chemistry* / Q000627:therapeutic use*; D002138:Calibration; D002243:Carbolines / Q000737:chemistry* / Q000627:therapeutic use*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D019587:Dietary Supplements / Q000032:analysis*; D005260:Female; D006801:Humans; D020018:Sexual Dysfunctions, Psychological / Q000188:drug therapy*; D000068581:Tadalafil; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000336:Aerosols; D001562:Benzimidazoles; D002243:Carbolines; C098107:flibanserin; D000068581:Tadalafil
keywords: Adulteration; Charged aerosol detector; Counterfeit herbal supplement; Flibanserin; Unified calibration