Simultaneous determination of sildenafil, vardenafil and tadalafil as forbidden components in natural dietary supplements for male sexual potency by high-performance liquid chromatography-electrospray ionization mass spectrometry

J Chromatogr A. 2005 Feb 25;1066(1-2):89-95. doi: 10.1016/j.chroma.2005.01.038.

Abstract

A high-performance liquid chromatographic method coupled with ultraviolet detection and electrospray ionization mass spectrometry (HPLC-UV-ESI-MS) was developed for simultaneous determination of banned additives-sildenafil, vardenafil and tadalafil in dietary supplements for male sexual potency. The separation was achieved on a C18 column with acetonitrile and aqueous solution (20 mmol ammonium acetate, 0.2% formic acid) as mobile phase at a flow rate of I ml/min with a linear gradient program. UV detection was at 292 nm. Identification of drugs was accomplished using ESI-MS. Good linearity between response (peak area) and concentration was found over a concentration range of 0.8-80 microg/ml for sildenafil; 2.25-225 microg/ml for vardenafil; and 1.1-110 microg/ml for tadalafil, with regression coefficient is better than 0.999. The recovery of the method ranged from 93.3 to 106.1%, and the relative standard deviation varied from 2.0 to 5.6% (n = 6). The method has been successfully applied to the analysis of practical samples of natural dietary supplements.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbolines / analysis*
  • Chromatography, High Pressure Liquid
  • Dietary Supplements / analysis*
  • Drug Contamination*
  • Imidazoles / analysis*
  • Phosphodiesterase Inhibitors / analysis*
  • Piperazines / analysis*
  • Purines
  • Sildenafil Citrate
  • Spectrometry, Mass, Electrospray Ionization
  • Sulfones / analysis*
  • Tadalafil
  • Triazines / analysis*
  • Vardenafil Dihydrochloride

Substances

  • Carbolines
  • Imidazoles
  • Phosphodiesterase Inhibitors
  • Piperazines
  • Purines
  • Sulfones
  • Triazines
  • Vardenafil Dihydrochloride
  • Tadalafil
  • Sildenafil Citrate