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Research Article Open access CC BY 4.0

Development of a Robust Method for Screening PDE-5 Inhibitor Additives in Dietary Supplements Using UPLC-MS/MS

Hua Wang

Asian Journal of Applied Chemistry Research · pp. 23–33 · Published 9 Dec 2023

10.9734/ajacr/2023/v14i4274

Abstract

A novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method was developed to detect the illegal additive of phosphodiesterase type 5 (PDE-5) inhibitors in dietary supplements. With the optimized chromatographic program, vardenafil, sildenafil, and tadalafil were separated within 5 minutes. The MS1, MS2, and retention time of PDE-5 inhibitors were acquired simultaneously within the information dependent acquisition mass spectrometry mode. Quantification was achieved via the quantity ion current chromatogram that was extracted from the total ion current. The linear range of vardenafil and sildenafil was 0.5-48 mg/L while the range of tadalafil was 0.3-36 mg/L. The correlation coefficients of the calibration curves of three PDE-5 inhibitors were all greater than 99.9%. At three concentration levels, the RSD values of the five repeat tests were all better than 1.30%. Sildenafil was detected in one dietary supplement. The comprehensive method of this study is reliable and may be a powerful tool for routine PDE-5 inhibitor screening and determination.

PDE-5 inhibitor illegal additive dietary supplements tandem mass spectrometry

References (33)

  1. 1 A critical review on the use of modern sophisticated hyphenated tools in the characterization of impurities and degradation products [DOI]
  2. 2 Oral Phosphodiesterase-5 Inhibitors and Hormonal Treatments for Erectile Dysfunction: A Systematic Review and Meta-analysis [DOI]
  3. 3 Phosphodiesterase 5 (PDE5): Structure-function regulation and therapeutic applications of inhibitors [DOI]
  4. 4 Therapeutic drug monitoring and LC–MS/MS [DOI]
  5. 5 Screening of synthetic PDE-5 inhibitors and their analogues as adulterants: Analytical techniques and challenges [DOI]
  6. 6 Phosphodiesterase‐5 Inhibitors: Action on the Signaling Pathways of Neuroinflammation, Neurodegeneration, and Cognition [DOI]
  7. 7 Use of liquid chromatography–mass spectrometry and a hydrolytic technique for the detection and structure elucidation of a novel synthetic vardenafil designer drug added illegally to a “natural” herbal dietary supplement [DOI]
  8. 8 Adulteration of herbal sexual enhancers and slimmers: The wish for better sexual well-being and perfect body can be risky [DOI]
  9. 9 Multiresidue Pesticide Analysis in Fresh Produce by Capillary Gas Chromatography−Mass Spectrometry/Selective Ion Monitoring (GC-MS/SIM) and −Tandem Mass Spectrometry (GC-MS/MS)† [DOI]
  10. 10 Accurate mass measurement using Fourier transform ion cyclotron resonance mass spectrometry for structure elucidation of designer drug analogs of tadalafil, vardenafil and sildenafil in herbal and pharmaceutical matrices [DOI]
  11. 11 Vision Disorders and Phosphodiesterase Type 5 Inhibitors [DOI]
  12. 12 Selective phosphodiesterase-5 (PDE-5) inhibitor vardenafil ameliorates renal damage in type 1 diabetic rats by restoring cyclic 3′,5′ guanosine monophosphate (cGMP) level in podocytes [DOI]
  13. 13 Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines [DOI]
  14. 14 Qualitative and quantitative analysis of PDE-5 inhibitors in counterfeit medicines and dietary supplements by HPLC–UV using sildenafil as a sole reference [DOI]
  15. 15 Monitoring by LC-MS/MS of 48 compounds of sildenafil, tadalafil, vardenafil and their analogues in illicit health food products in the Korean market advertised as enhancing male sexual performance [DOI]
  16. 16 Analysis of phosphodiesterase type 5 inhibitors as possible adulterants of botanical-based dietary supplements: extensive survey of preparations available at the Czech market [DOI]
  17. 17 Phosphodiesterase type 5 inhibitors and kidney disease [DOI]
  18. 18 Characterization of Sildenafil analogs by MS/MS and NMR: A guidance for detection and structure elucidation of phosphodiesterase-5 inhibitors [DOI]
  19. 19 The efficacy of PDE5 inhibitors in diabetic patients [DOI]
  20. 20 LC-MS/MS method for the quantitation of serum tocilizumab in rheumatoid arthritis patients using rapid tryptic digestion without IgG purification [DOI]
  21. 21 Advanced hydrogels: New expectation for the repair of organic erectile dysfunction [DOI]
  22. 22 Phosphodiesterase-5 inhibitors and their analogues as adulterants of herbal and food products: analysis of the Malaysian market, 2014–16 [DOI]
  23. 23 Multiple Reaction Monitoring with Multistage Fragmentation (MRM3) Detection Enhances Selectivity for LC-MS/MS Analysis of Plasma Free Metanephrines [DOI]
  24. 24 Reliable screening and classification of phosphodiesterase type 5 inhibitors in dietary supplements using gas chromatography / mass spectrometry combined with specific common ions [DOI]
  25. 25 Determination of Analogs of Sildenafil and Vardenafil in Foods by Column Liquid Chromatography with a Photodiode Array Detector, Mass Spectrometry, and Nuclear Magnetic Resonance Spectrometry [DOI]
  26. 26 Structural elucidation of a PDE-5 inhibitor detected as an adulterant in a health supplement [DOI]
  27. 27 Development and validation of an ultra-high performance liquid chromatography-high resolution mass spectrometry method for simultaneous quantification of cyanogenic glycosides and secoisolariciresinol diglucoside in flaxseed (Linum usitatissimum L.) [DOI]
  28. 28 Single Analyzer Neutral Loss Scans in a Linear Quadrupole Ion Trap Using Orthogonal Double Resonance Excitation [DOI]
  29. 29 The paradigm shifting role of chromatographic methods in pharmaceutical analysis [DOI]
  30. 30 Screening of Phosphodiesterase-5 Inhibitors and Their Analogs in Dietary Supplements by Liquid Chromatography–Hybrid Ion Trap–Time of Flight Mass Spectrometry [DOI]
  31. 31 Cyclic guanosine monophosphate modulates accumulation of phosphodiesterase 5 inhibitors in human platelets [DOI]
  32. 32 Dispersive magnetic solid-phase extraction for synthetic PDE-5 inhibitors determination by high-performance liquid chromatography with tandem mass spectrometry [DOI]
  33. 33 Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization [DOI]

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