Determination of Phosphodiesterase Type 5 Enzyme (PDE-5) Inhibitors and Analogues as Adulterants in Selected Herbal Products using Gas Chromatography–Electron Impact-Mass Spectrometer (GC-EI-MS)

Abstract

Sildenafil, tadalafil, and vardenafil are phosphodiesterase type 5 enzyme (PDE-5) inhibitors used for the treatment of male erectile dysfunction. This present study aims to investigate 55 herbal products indicated for men’s sexual health from the Malaysian market for adulteration of PDE-5 inhibitors and analogues. The screening and identification of 20 PDE-5 inhibitors and analogues in herbal products of various forms (powder, capsules, tablets, and pastels) were conducted using gas chromatography–electron impact-mass spectrometer (GC-EI-MS). The analysis has shown that 19 herbal products were adulterated with PDE-5 inhibitors and analogues. Unique ion fragmentations and the presence of molecular ion serve as potential markers, and the limit of detection (LOD) was 0.1-5.0 µg/g. Ten PDE-5 inhibitors and analogues were randomly selected and successfully validated for simultaneous quantification, whereby the limit of quantitation (LOQ) was 5.0–50.0 µg/g with recoveries at 86.1-118.9%. The developed method of GC-EI-MS was shown to be simple, throughput, economical and had sufficient sensitivity to screen, identify and quantify PDE-5 inhibitors and analogues in herbal matrices.

Optimization and Validation of HPLC-UV Method for the Determination of Vardenafil, Sildenafil, and Tadalafil in Honey-Mixed Herbal Sachets Using a Design of Experiment

“…In this case, various spectroscopic and chromatographic methods are used to inspect illegally grown foods containing undeclared synthetic drugs in a complex matrix. The most common techniques for measuring PDE5 inhibitors and their analogs are UV-Vis detectors (UVs) [21][22][23], spectrophotometers [24], and gas chromatography combined with mass spectrometry (High-Performance Liquid Chromatography (HPLC) with GC-MS) [25]. Recently, liquid chromatography (LC-MS) combined with mass spectrometry and liquid chromatography (LC-MS / MS) combined with tandem mass spectrometry have been adopted [19,[26][27][28].…”