Article ID Journal Published Year Pages File Type
1200013 Journal of Chromatography A 2014 8 Pages PDF
Abstract

•Simultaneous qualitative and quantitative analysis of eleven PDE-5 inhibitors.•Q-Orbitrap HRMS in full MS/dd-MS2 mode was used for screening of illegal adulterants.•Good linearity, accuracy, precision and selectivity were observed upon HRMS analysis.•Illegal adulterated sildenafil and noracetildenafil were detected in 9 dietary supplements.

In this study, the applicability of high resolution quadrupole-Orbitrap (Q-Orbitrap) mass spectrometry for the simultaneous qualitative and quantitative analysis of illegal adulterated phosphodiesterase-5 inhibitors (PDE-5 inhibitors) in herbal medicines and dietary supplements was investigated. The mass spectrometer was operated in full MS scan/dd-MS2 (data-dependent MS2) mode. The use of 70 000 FWHM mass resolution and narrow mass windows (5 ppm) could effectively improve the selectivity of the method, increasing the signal-to-noise ratio for the analytes. The response showed good linear relationship with the analytes’ concentrations over wide ranges (e.g., 0.05–10 μg/g for sildenafil) with all the coefficient of determinations (r2) >0.9996. The detection limits (LODs) were in the range of 1.0–5.0 ng/g for different analytes. The recoveries ranged from 85.4% to 96.7%. The intra- and inter-day accuracies were in the range of −6.6 to 10.1%, while the intra- and inter-day precision ranged from 0.0039% to 13.2%. Among 68 batches of herbal medicines and 20 batches of dietary supplements (including 83 capsules, 3 pellets and 2 liquid) samples, sildenafil was detected in 8 dietary supplements, while noracetildenafil was detected in only one dietary supplement. The novel Q-Orbitrap mass spectrometry has been proved to be a very promising and powerful tool for routine screening of illegal adulterate in herbal medicines and dietary supplements, ensuring food safety and public health.

Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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