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.
abstract: 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 10mM 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.
authors.affiliation: Laboratory of Drug Analysis, Scientific Institute of Public Health, Brussels, Belgium.
authors.forename: Pierre-Yves
authors.initials: PY
authors.lastname: Sacré
authors.forename: Eric
authors.initials: E
authors.lastname: Deconinck
authors.forename: Patrice
authors.initials: P
authors.lastname: Chiap
authors.forename: Jacques
authors.initials: J
authors.lastname: Crommen
authors.forename: François
authors.initials: F
authors.lastname: Mansion
authors.forename: Eric
authors.initials: E
authors.lastname: Rozet
authors.forename: Patricia
authors.initials: P
authors.lastname: Courselle
authors.forename: Jacques O
authors.initials: JO
authors.lastname: De Beer
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000704:Analysis of Variance; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D058110:Counterfeit Drugs / Q000032:analysis / Q000737:chemistry*; D016014:Linear Models; D058986:Phosphodiesterase 5 Inhibitors / Q000032:analysis / Q000737:chemistry*; D010879:Piperazines / Q000032:analysis / Q000737:chemistry; D011687:Purines / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D000068677:Sildenafil Citrate; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D013450:Sulfones / Q000032:analysis / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D058110:Counterfeit Drugs; D058986:Phosphodiesterase 5 Inhibitors; D010879:Piperazines; D011687:Purines; D013450:Sulfones; D000068677:Sildenafil Citrate; C032159:acetonitrile