Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines
[en] Pharmaceutical counterfeiting is a permanently growing problem. Control laboratories are constantly analysing counterfeit medicines. In industrialised countries, one of the main counterfeited class of medicines are erectile dysfunction drugs. This paper describes the development and validation of a fast method to detect and quantify the three authorised phosphodiesterase type 5 inhibitors and five analogues. The method is based on the use of a sub-2 microns polar-embedded column with a gradient using acetonitrile as organic modifier and 10 mM ammonium formate buffer (pH 3.5) as aqueous component of the mobile phase. The separation was achieved in less than 4.5 min. The method has also been compared to the registered HPLC method for the assay of Viagra® which was considered as the reference method.
The method is also compatible with on-line coupling mass spectrometry and will significantly reduce analysis times and solvent consumption.
Research Center/Unit :
Centre Interfacultaire de Recherche du Médicament - CIRM
Chiap, Patrice ; Université de Liège - ULiège > Département de pharmacie > Département de pharmacie
Crommen, Jacques ; Université de Liège - ULiège > Département de pharmacie > Département de pharmacie
Mansion, François ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Courselle, Patricia
De Beer, Jacques
Language :
English
Title :
Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines
B.J. Venhuis, D.M. Barends, M.E. Zwaagstra, D. de Kaste, Recent developments in counterfeit and imitations of Viagra, Cialis and Levitra, RIVM Report 370030001/2007, Bilthoven, 2007.
Lee H.M., Kim C.S., Jang Y.M., Kwon S.W., Lee B.J. J. Pharm. Biomed. Anal. 2011, 54:491.
Singh S., Prasad B., Savaliya A., Shah R., Gohil V., Kaur A. Trends Anal. Chem. 2009, 28:13.
Gratz S., Zeller M., Mincey D., Flurer C. J. Pharm. Biomed. Anal. 2009, 50:228.
Reepmeyer J., d'Avignon D.A. J. Pharm. Biomed. Anal. 2009, 49:145.
Lin M.C., Liu Y.C., Lin J.H. J. Food Drug Anal. 2006, 14:260.
Lai K.C., Liu Y.C., Tseng M.C., Lin J.H. J. Food Drug. Anal. 2006, 14:19.
Hou P., Zou P., Low M.Y., Chan E., Koh H.L. Food Addit. Contam. A 2006, 23:870.
Shin C., Hong M., Kim D., Lim Y. Magn. Reson. Chem. 2004, 42:1060.
Blok-Tip L., Zomer B., Bakker F., Hartog K.D., Hamzink M., ten Hove J., Vredenbregt M., de Kaste D. Food Addit. Contam. A 2004, 21:737.
Nagaraju V., Sreenath D., Tirumala Rao J., Nageswara Rao R. Anal. Sci. 2003, 19:1007.
Dinseh N.D., Vishukumar B.K., Nagaraja P., Made Gowda N.M., Rangappa K.S. J. Pharm. Biomed. Anal. 2002, 29:743.
Daragmeh N., Al-Omari M., Badwan A.A., Jaber A.M.Y. J. Pharm. Biomed. Anal. 2001, 25:483.
Häberli A., Girard P., Low M.Y., Gei X. J. Pharm. Biomed. Anal. 2010, 53:24.
Venhuis B.J., Zomer G., Vredenbregt M.J., de Kaste D. J. Pharm. Biomed. Anal. 2010, 51:723.
Aboul-Enein H.Y., Ali I. Talanta 2005, 65:276.
Reepmeyer J.C., Woodruff J.T. J. Chromatogr. A 2006, 1125:67.
De Orsi D., Pellegrini M., Marchei E., Nebuloni P., Gallinella B., Scaravelli G., Martufi A., Gagliardi L., Pichini S. J. Pharm. Biomed. Anal. 2009, 50:362.
Gryniewicz C.M., Reepmeyr J.C., Kauffman J.F., Buhse L.F. J. Pharm. Biomed. Anal. 2009, 49:601.
Savalyia A.A., Shah R.P., Prasad B., Singh S. J. Pharm. Biomed. Anal. 2010, 52:406.
Choi D.M., Park S., Yoon T.H., Jeong H.K., Pyo J.S., Park J., Kim D., Kwon S.W. J. AOAC Int. 2008, 91:580.
Park H.J., Jeong H.K., Chang M.I., Im M.H., Jeong J.Y., Choi D.M., Park K., Hong M.K., Youm J., Han S.B., Kim D.J., Park J.H., Kwon S.W. Food Addit. Contam. 2007, 24:122.
ISO/IEC 17025 General requirements for the competence of testing and calibration laboratories 2005, ISO, Geneva.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Chiap P., Cohen N., Compagnon P.A., Dewé W., Feinberg M., Lallier M., Laurentie M., Mercier N., Muzard G., Nivet C., Valat L. J. Pharm. Biomed. Anal. 2004, 36:579.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Chiap P., Cohen N., Compagnon P.A., Dewé W., Feinberg M., Lallier M., Laurentie M., Mercier N., Muzard G., Nivet C., Valat L., Rozet E. J. Pharm. Biomed. Anal. 2007, 45:70.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Cohen N., Compagnon P.A., Dewé W., Feinberg M., Laurentie M., Mercier N., Muzard G., Valat L., Rozet E. J. Pharm. Biomed. Anal. 2007, 45:82.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Cohen N., Compagnon P.A., Dewé W., Feinberg M., Laurentie M., Mercier N., Muzard G., Valat L., Rozet E. J. Pharm. Biomed. Anal. 2008, 48:760.
Feinberg M., Boulanger B., Dewé W., Hubert Ph. Anal. Bioanal. Chem. 2004, 380:502.
Feinberg M. J. Chromatogr. A 2007, 1158:174.
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., Hubert Ph. J. Chromatogr. A 2007, 1158:111.
Araujo P. J. Chromatogr. B 2009, 877:2224.
Horwitz W., Albert R. J. AOAC Int. 2006, 89:1095.
Massart D.L., Vandeginste B.G.M., Buydens L.M.C., De Jong S., Lewi P.J., Smeyers-Verbeke J. Handbook of Chemometrics and Qualimetrics: Part A 1997, Elsevier Science, Amsterdam.
