Rapid Screening and Identification of Illegally Adulterated PDE-5 Inhibitors in Health Wines by UPLC-TOF-MS
Health wines are alcoholic beverages produced by infusing traditional liquors or rice wines with natural, medicinal, and food-safe ingredients. However, to accelerate efficacy, some manufacturers illegally adulterate health wines with phosphodiesterase type 5 (PDE-5) inhibitors, which may cause severe adverse effects. This study developed a method based on ultra-high-performance liquid chromatography–time-of-flight mass spectrometry (UPLC–TOF/MS) for the rapid screening and identification of 68 PDE-5 inhibitors illegally added to health wines. After optimizing the sample preparation procedure, chromatographic conditions, mass spectrometric parameters, and primary and secondary mass spectra of the 68 PDE-5 inhibitors were acquired as reference standards. Retention times and mass spectral data were imported into the Personal Compound Database and Library, establishing a high-resolution screening database with matched drug names, molecular formulas, and accurate molecular weights. A quantitative method was validated using 11 commonly adulterated compounds, including sildenafil. The response was highly linear (r ≥ 0.9988; 0.8–400 μg/L) with low detection limits (0.2–1.0 μg/L). The average spiked recoveries were 71.2–104.1%, with relative standard deviations of ≤10.1%. Among 59 commercial health wine samples, three batches tested positive for PDE-5 inhibitors (detection rate: 5.1%). The proposed method can assist market surveillance even when reference standards are unavailable for all compounds.
Authors
- Yun Du (ORCID: https://orcid.org/0000-0002-0711-3919)
- Xiaobei Huang
- Yuli Fu
- Zi Yi (ORCID: https://orcid.org/0000-0003-4588-9846)
- Ben Li
- Hui Wang (ORCID: https://orcid.org/0000-0003-2791-8981)
- Lixia Yang (ORCID: https://orcid.org/0000-0003-2093-8445)
Institutions
- Hunan Normal University (CN)
- Hunan Provincial Center for Disease Control and Prevention (CN)
- Shandong Institute of Food and Drug Inspection (CN)
Publication Details
- Journal
- Processes
- Published
- 2025-11-25
- DOI
- https://doi.org/10.3390/pr13123800
- Primary Topic
- Pharmaceutical Quality and Counterfeiting
- Type
- article
- Field-Weighted Citation Impact
- 0.00
Funders
- National Natural Science Foundation of China
- Natural Science Foundation of Hunan Province