Development of a comprehensive spectral library of sildenafil and related active analogues using LC–QTOF–MS and its application for screening counterfeit pharmaceuticals. (December 2015)

• Record Type: Journal Article
• Authors: Lee, Sooyeun; Ji, Dajeong; Park, Meejung; Chung, Kyu Hyuck
• Is Part Of: Forensic science international. Volume 257(2015)
• Page Start: 182
• Page End: 188
• Publication Date: 2015-12
• Subjects: Spectral library -- Sildenafil -- Counterfeit drugs -- LC–QTOF–MS; Medical jurisprudence -- Periodicals; Chemistry, Forensic -- Periodicals; Forensic Medicine -- Periodicals; Médecine légale -- Périodiques; Chimie légale -- Périodiques; Gerechtelijke geneeskunde; Gerechtelijke chemie; Gerechtelijke psychiatrie; Chemistry, Forensic; Medical jurisprudence; Electronic journals; Periodicals; Electronic journals; 614.1
• DOI: 10.1016/j.forsciint.2015.08.016
• Languages: English
• ISSNs: 0379-0738

Abstract

Highlights: An LC–QTOF–MS spectral library of 40 sildenafil analogues was developed. The library consisted of ion fragmentation patterns and retention times. This in-house library successfully detected counterfeit pharmaceuticals. Abstract: The abuse or misuse of forged erectile-dysfunction drugs, containing phosphodiesterase type 5 inhibitors (e.g. sildenafil), is a serious issue globally. Therefore, the detection of sildenafil and related active analogues in counterfeit pharmaceuticals or the differentiation between counterfeit and authentic drugs has been performed with a variety of analytical techniques. Recently, a liquid chromatography–hybrid quadrupole time-of-flight mass spectrometry (LC–QTOF–MS)-based in-house library, consisting of accurate mass ion fragmentation information and retention times, was effectively applied to screen a large number of compounds in field of forensic toxicology. However, a comprehensive LC–QTOF–MS spectral library of sildenafil and related active analogues has not yet been reported. In the present study, a spectral library of 40 compounds of sildenafil and related analogues was developed with accurate mass spectra and retention times using LC–QTOF–MS, and applied to screen nine marketed counterfeit products. The in-house library successfully identified sildenafil, dimethylsildenafil, hydroxyhomosildenafil, demethylhongdenafil, pseudovardenafil and vardenafil in the samples. Our LC–QTOF–MS-based spectral library search is considered a powerful approach for identifying sildenafil and related active analogues in counterfeit pharmaceuticals.