Improved QuEChERS-LC-MS/MS Method for the Detection and Quantification of Tadalafil, Sildenafil, and Vardenafil in Dietary Supplements
نویسندگان
1 TSL Science Co., Lot II-12A, 19/5A Street, Cluster 4, Industrial Group II, Tan Binh Industrial Zone, Tan Phu District, Ho Chi Minh City
2 Faculty of Chemical Engineering, Industrial University of Ho Chi Minh City, 12 Nguyen Van Bao, Go Vap, Ho Chi Minh City 700000, Vietnam
3 Faculty of Chemical Engineering, Industrial University of Ho Chi Minh City, 12 Nguyen Van Bao, Go Vap, Ho Chi Minh City 700000, Vietnam
4 Faculty of Chemical Engineering, Industrial University of Ho Chi Minh City, 12 Nguyen Van Bao, Go Vap, Ho Chi Minh City 700000, Vietnam
5 Institue of Biotechnology and Food Technology, Industrial University of Ho Chi Minh City, 12 Nguyen Van Bao Street, Ward 1, Go Vap District, Ho Chi Minh City 700000, Viet Nam
doi
10.22036/abcr.2026.559103.2475چکیده
The unauthorized adulteration of dietary supplements with phosphodiesterase type 5 (PDE5) inhibitors poses significant public health risks. This study presents a rapid, sensitive, and accurate analytical method for the simultaneous determination of Tadalafil, Sildenafil, and Vardenafil using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction technique coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction procedure was optimized using acetonitrile containing 1% ammonium acetate as the solvent, followed by a dispersive solid-phase extraction (d-SPE) clean-up step utilizing PSA, C18, and MgSO4. The method was validated according to AOAC guidelines, demonstrating excellent linearity (R² > 0.9991), low limits of detection (LOD) ranging from 0.18 to 0.98 µg/kg, and recoveries between 81.3% and 105.2% with relative standard deviations (RSD) below 15%. The applicability of the method was confirmed through the analysis of twelve commercial dietary supplements, revealing one tablet sample adulterated with Tadalafil (71.1 mg/kg), Sildenafil (46.4 mg/kg), and Vardenafil (25.5 mg/kg). These results indicate that the developed method is highly effective for the regulatory monitoring and quality control of functional foods.
