Identification of Descarbonsildenafil in an Adulterated Dietary Supplement and Evaluation of Its Inhibitory Activity for Phosphodiesterase Type 5 (PDE5)

Development of a detector tube for screening tadalafil and its analogues in adulterated sexual enhancement products

“…Samples showing a peak presumed to be attributed to PDE‐5i, as detected by LC–PDA analyses, were subsequently analyzed by LC–MS/MS analyses performed on an ACQUITY UPLC® (Waters Corporation) and TQD (Waters Corporation) using an ACQUITY UPLC® HSS C18 column (2.1 × 150 mm i.d., particle size: 1.8 μm, Waters Corporation) at 50°C. The composition of a mobile phase with formic acid‐acetonitrile and the mode of gradient elution of the analyses were identical to those reported previously 26 . The MS/MS conditions were as follows: electrospray ionization (ESI) negative mode (Td, homotadalafil, aminotadalafil, and chloropretadalafil) and ESI positive mode (the others); scan range, m/z 50–550; capillary, 3.0 kV; desolvation temperature, 400°C; source temperature, 150°C; cone gas flow (nitrogen), 20 L/h; desolvation gas flow (nitrogen), 800 L/h; cone voltage, 20 V (dimetyldithiodenafil) or 40 V (the others); and collision energy, 5–30 eV (Td, homotadalafil, aminotadalafil, and chloropretadalafil) or 10–60 eV (the others).…”

“…LC–PDA analyses were performed on an ACQUITY UPLC® HSS C18 column (2.1 × 150 mm i.d., particle size: 1.8 μm, Waters Corporation Milford, MA, USA) at 50°C. Measurements were carried out under gradient elution mode, with a mobile phase of acetonitrile containing sodium 1‐hexanesulfonic acid sodium salt, as has been previously reported 26 …”