title: High performance liquid chromatography-diode array and electrospray-mass spectrometry analysis of vardenafil, sildenafil, tadalafil, testosterone and local anesthetics in cosmetic creams sold on the Internet web sites.
abstract: A simple high-performance liquid chromatography (HPLC) method with ultraviolet diode array (UV-DAD) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of vardenafil, sildenafil, tadalafil, testosterone, procaine, lidocaine, prilocaine, and benzocaine in cosmetic creams sold as promising remedies for male erectile dysfunction and female genitals stimulation. The presence of these substances in commercial cosmetic samples is prohibited. Aliquots (1 g) of the cosmetic creams under investigation were diluted 1:100 in methanol, subjected to ultrasonic treatment, added with benzoic acid as internal standard, and analyzed by HPLC-DAD and HPLC-ESI-MS after a further 1:1000 dilution. The compounds were separated by reversed phase chromatography with water (0.02% trifluoroacetic acid) and acetonitrile gradient elution and detected by UV-DAD at 228, 255 and 290 nm and by ESI-MS positive ionisation mode. Benzoic acid was used as internal standard. Linearity was studied with UV-DAD detection from 2.5-7.8 to 250 microg/g range, depending on the different compounds and with ESI-MS in the 3.3-8.9 to 250 ng/g range. Good determination coefficients (r(2) > or = 0.99) were found in both UV-DAD and ESI-MS. Limits of quantifications ranged between 2.5 and 7.8 microg/g for HPLC-UV-DAD assay and between 3.3 and 8.9 ng/g for HPLC-ESI-MS assay depending on different analyzed substances. At three concentrations spanning the linear dynamic ranges of both UV-DAD and ESI-MS assay, mean recoveries were always higher than 90% for the different analytes and intra-assay and inter-assay precision always better than 15% and 12%. This method was successfully applied to the analysis of substances under investigations present in cosmetic creams, freely sold on the Internet web-sites.
authors.affiliation: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanità, V.le Regina Elena 299, 00161, Rome, Italy.
authors.forename: Daniela
authors.initials: D
authors.lastname: De Orsi
authors.forename: Manuela
authors.initials: M
authors.lastname: Pellegrini
authors.forename: Emilia
authors.initials: E
authors.lastname: Marchei
authors.forename: Paolo
authors.initials: P
authors.lastname: Nebuloni
authors.forename: Bruno
authors.initials: B
authors.lastname: Gallinella
authors.forename: Giulia
authors.initials: G
authors.lastname: Scaravelli
authors.forename: Alessio
authors.initials: A
authors.lastname: Martufi
authors.forename: Luigi
authors.initials: L
authors.lastname: Gagliardi
authors.forename: Simona
authors.initials: S
authors.lastname: Pichini
mesh_terms: D000779:Anesthetics, Local / Q000032:analysis*; D002243:Carbolines / Q000032:analysis; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003358:Cosmetics; D005260:Female; D006801:Humans; D007093:Imidazoles / Q000032:analysis; D020407:Internet; D008297:Male; D010726:Phosphodiesterase Inhibitors / Q000032:analysis*; D010879:Piperazines / Q000032:analysis; D011687:Purines / Q000032:analysis; D015203:Reproducibility of Results; D000068677:Sildenafil Citrate; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013450:Sulfones / Q000032:analysis; D000068581:Tadalafil; D013739:Testosterone / Q000032:analysis; D014227:Triazines / Q000032:analysis; D000069058:Vardenafil Dihydrochloride
chemical_list: D000779:Anesthetics, Local; D002243:Carbolines; D003358:Cosmetics; D007093:Imidazoles; D010726:Phosphodiesterase Inhibitors; D010879:Piperazines; D011687:Purines; D013450:Sulfones; D014227:Triazines; D013739:Testosterone; D000069058:Vardenafil Dihydrochloride; D000068581:Tadalafil; D000068677:Sildenafil Citrate