Simultaneous Determination of Sildenafil, Vardenafil, and Tadalafil in Health Foods by Ultra-performance Liquid Chromatography Tandem Mass Spectrometry
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Abstract:
A method was established for the determination of vardenafil, sildenafil, and tadalafil in health foods using solid-phase extraction–ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The sample was extracted by methanol or hydrochloric acid, and then purified by a hydrophilic/lipophilic balanced (HLB) SPE column. The target compounds were separated on a reversed phase column using a solution of acetonitrile and 0.1 % formic acid in water as the mobile phase, and then detected by positive electrospray ionization under multiple reaction monitoring (MRM) mode. Good linearity of the calibration curves was achieved for three target compounds in the range of 10 ~200 μg/L, with correlation coefficients (r2) greater than 0.99. The average recoveries of the blank matrix sample were all more than 75%, and the relative standard deviations (RSDs) were less than 8%. The limits of detection (LOD) for vardenafil, sildenafil, and tadalafil in the capsule form were 10 μg/kg, 10 μg/kg, and 20 μg/kg, respectively. The limits of quantitation (LOQs) for vardenafil, sildenafil, and tadalafil in the capsule form were 40 μg/kg, 40 μg/kg, and 80 μg/kg, respectively. For oral samples, the LODs were 3 μg/L, 3 μg/L, and 6 μg/L, respectively; the LOQs were 10 μg/L, 10 μg/L, and 20 μg/L, respectively. The sample matrix effects were also studied, which had a suppressive effect on the response of vardenafil, sildenafil, and tadalafil, and the most significant suppressive effect was found on vardenafil.
