title: Application of a high resolution benchtop quadrupole-Orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietary supplements.
abstract: 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-MS(2) (data-dependent MS(2)) 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 (r(2)) >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.
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Feng
authors.initials: F
authors.lastname: Shi
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China. Electronic address: gcc007@163.com.
authors.forename: Changchuan
authors.initials: C
authors.lastname: Guo
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Liping
authors.initials: L
authors.lastname: Gong
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Jun
authors.initials: J
authors.lastname: Li
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Peng
authors.initials: P
authors.lastname: Dong
authors.affiliation: Cancer Center, Linyi's People Hospital, Linyi 276000, PR China. Electronic address: jinlingzhang_931@163.com.
authors.forename: Jinling
authors.initials: J
authors.lastname: Zhang
authors.affiliation: Service team, Thermo Fisher Scientific, Beijing 100007, PR China.
authors.forename: Ping
authors.initials: P
authors.lastname: Cui
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Shuyin
authors.initials: S
authors.lastname: Jiang
authors.affiliation: Shandong Institute for Food and Drug Control, Jinan, Shandong 250101, PR China.
authors.forename: Yanxia
authors.initials: Y
authors.lastname: Zhao
authors.affiliation: Lab of Pharmaceutical Analysis and Drug Metabolism, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, Zhejiang 310058, PR China.
authors.forename: Su
authors.initials: S
authors.lastname: Zeng
mesh_terms: D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D029001:Herbal Medicine; D013058:Mass Spectrometry / Q000379:methods; D058986:Phosphodiesterase 5 Inhibitors / Q000032:analysis*; D010879:Piperazines / Q000032:analysis; D010936:Plant Extracts / Q000737:chemistry*; D011687:Purines / Q000032:analysis; D000068677:Sildenafil Citrate; D013450:Sulfones / Q000032:analysis
chemical_list: D058986:Phosphodiesterase 5 Inhibitors; D010879:Piperazines; D010936:Plant Extracts; D011687:Purines; D013450:Sulfones; D000068677:Sildenafil Citrate
keywords: Illegal adulteration; Orbitrap; Phosphodiesterase-5 inhibitors; Qualitation; Quantitation; Screening