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25 November 2025

15 Pages

Rapid Screening and Identification of Illegally Adulterated PDE-5 Inhibitors in Health Wines by UPLC-TOF-MS

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1
Changsha Institute for Food and Drug Control, National Alcohol Products Quality Supervision and Inspection Center, Changsha 410013, China
2
Key Laboratory of the Assembly and Application of Organic Functional Molecules, Hunan Normal University, Changsha 410081, China
3
Changsha Center for Diseases Prevention and Control, Changsha 410004, China
*
Author to whom correspondence should be addressed.
This article belongs to the Section Food Process Engineering

Abstract

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.

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