Back to Search
Start Over
Analysis of phosphodiesterase type 5 inhibitors as possible adulterants of botanical-based dietary supplements: extensive survey of preparations available at the Czech market.
- Source :
-
Journal of pharmaceutical and biomedical analysis [J Pharm Biomed Anal] 2019 Feb 05; Vol. 164, pp. 713-724. Date of Electronic Publication: 2018 Nov 03. - Publication Year :
- 2019
-
Abstract
- Popularity of natural-based preparations supporting the sexual potency significantly increased in recent years, which also led to the increase of illegal use of phosphodiesterase type 5 inhibitor (PDE-5) in sexual performance enhancement products. In this study, a rapid U-HPLC‒HRMS/MS method has been developed to simultaneously determine 59 PDE-5 inhibitors and their analogues. Within the development of sensitive method for analysis of 59 PDE-5 inhibitors and their analogues, both sample preparation procedure, as well as separation / detection conditions have been optimized. Extraction efficiency of particular extraction solvents, influence of different mobile phase additives on target analytes separation, as well as impact of various settings of mass analyzer on sensitivity of detection were examined. Data were collected in the 'full MS/data dependent MS/MS' acquisition mode (full MS-dd-MS/MS). Before the U-HPLC‒HRMS/MS method was used for analysis of real samples, proper validation had been conducted. The precision of the method expressed as the relative standard deviation (RSD) was ≤4.2% and ≤5.2% at spiking concentrations 5 μg/g and 0.25 μg/g, respectively. The limits of quantification were in the range 0.25 - 0.05 μg/g and the recovery ranged between 71 and 90%. The optimized method was successfully applied for analysis of 64 real samples, and 10 of them were proved to contain both registered or unregistered synthetic PDE-5 inhibitors. Additionally, the acquired U-HPLC‒HRMS/MS fingerprints were demonstrated to serve as an efficient tool for revealing of other type of possible fraud in products labeling. Retrospective mining of markers of herbs declared on dietary supplements packaging allowed to assess the trueness / untruth in the declaration of medical herbs composition.<br /> (Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.)
- Subjects :
- Chromatography, High Pressure Liquid methods
Czech Republic
Dietary Supplements analysis
Drug Contamination prevention & control
Limit of Detection
Phytochemicals analysis
Tandem Mass Spectrometry methods
Counterfeit Drugs analysis
Dietary Supplements standards
Fraud prevention & control
Phosphodiesterase 5 Inhibitors analysis
Phytochemicals standards
Subjects
Details
- Language :
- English
- ISSN :
- 1873-264X
- Volume :
- 164
- Database :
- MEDLINE
- Journal :
- Journal of pharmaceutical and biomedical analysis
- Publication Type :
- Academic Journal
- Accession number :
- 30472590
- Full Text :
- https://doi.org/10.1016/j.jpba.2018.11.007