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

被引:52
作者
De Orsi, Daniela [1 ]
Pellegrini, Manuela [1 ]
Marchei, Emilia [1 ]
Nebuloni, Paolo [2 ]
Gallinella, Bruno [1 ]
Scaravelli, Giulia [3 ]
Martufi, Alessio [2 ]
Gagliardi, Luigi [1 ]
Pichini, Simona [1 ]
机构
[1] Ist Super Sanita, Dept Therapeut Res & Med Evaluat, I-00161 Rome, Italy
[2] Waters Spa Italy, Surveillance & Hlth Promot, Ist Super Sanita, Rome, Italy
[3] Ist Super Sanita, Natl Ctr Epidemiol Surveillance & Hlth Promot, I-00161 Rome, Italy
关键词
Cosmetic creams; PDE-5; inhibitors; Testosterone; Local anaesthetics; HPLC-UV-DAD; ESI-MS; PHOSPHODIESTERASE TYPE-5 INHIBITORS; ERECTILE DYSFUNCTION; DIETARY-SUPPLEMENTS; EFFICACY; MEN;
D O I
10.1016/j.jpba.2009.05.022
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 mu g/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) >= 0.99) were found in both UV-DAD and ESI-MS. Limits of quantifications ranged between 2.5 and 7.8 mu g/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. (C) 2009 Elsevier B.V. All rights reserved.
引用
收藏
页码:362 / 369
页数:8
相关论文
共 17 条
[11]  
Gresser U, 2002, EUR J MED RES, V7, P435
[12]   Sustained efficacy and tolerability of vardenafil, a highly potent selective phosphodiesterase type 5 inhibitor, in men with erectile dysfunction: Results of a randomized, double-blind, 26-week placebo-controlled pivotal trial [J].
Hellstrom, WJG ;
Gittelman, M ;
Karlin, G ;
Segerson, T ;
Thibonnier, M ;
Taylor, T ;
Padma-Nathan, H .
UROLOGY, 2003, 61 (04) :8-14
[13]   Vision Disorders and Phosphodiesterase Type 5 Inhibitors A Review of the Evidence to Date [J].
Laties, Alan M. .
DRUG SAFETY, 2009, 32 (01) :1-18
[14]   Development of an HPLC method for the identification and dosage of non-allowed substances in cosmetic products.: Part I:: local anaesthetics and antihistaminics [J].
Porrà, R ;
Berri, S ;
Gagliardi, L ;
Chimenti, P ;
Granese, A ;
De Orsi, D ;
Carpani, I ;
Tonelli, D .
ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 2004, 380 (5-6) :767-772
[15]   PHOSPHODIESTERASE TYPE-5 INHIBITOR AND OXIDATIVE STRESS [J].
Speranza, L. ;
Franceschelli, S. ;
Pesce, M. ;
Vinciguerra, I. ;
De Lutiis, M. A. ;
Grilli, A. ;
Felaco, M. ;
Patruno, A. .
INTERNATIONAL JOURNAL OF IMMUNOPATHOLOGY AND PHARMACOLOGY, 2008, 21 (04) :879-889
[16]   Comparison of phosphodiesterase type 5 (PDE5) inhibitors [J].
Wright, P. J. .
INTERNATIONAL JOURNAL OF CLINICAL PRACTICE, 2006, 60 (08) :967-975
[17]   Simultaneous determination of synthetic phosphodiesterase-5 inhibitors found in a dietary supplement and pre-mixed bulk powders for dietary supplements using high-performance liquid chromatography with diode array detection and liquid chromatography-electrospray ionization tandem mass spectrometry [J].
Zou, P ;
Oh, SSY ;
Hou, PL ;
Low, MY ;
Koh, HL .
JOURNAL OF CHROMATOGRAPHY A, 2006, 1104 (1-2) :113-122