Determination of tadalafil andN-desmethylsibutramine in health and dietary supplements using ultra-performance liquid chromatography (UPLC) coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF MS)

Abstract

The adulteration of dietary supplements with drugs is potentially dangerous for human health. In this study, a method was used to test simultaneously for the presence of three synthetic PDE-5 inhibitors (sildenafil, vardenafil and tadalafil), and sibutramine and its two major metabolites (N-desmethylsibutramine and N-didesmethylsibutramine) using ultra-performance liquid chromatography (UPLC) coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF MS) in dietary supplements. This approach with UPLC/Q-TOF MS uses the high accurate mass of six compounds for identification and has a short run time. The recovery was from 87% to 113%; precision was less than 12.8%. The limit of detection and limit of quantification were from 0.4 to 2.0 µg kg(-1) and from 1.3 to 6.0 µg kg(-1), respectively. This method allows easy and fast analysis and detection of diverse adulterants.

Towards a decade of detecting new analogues of sildenafil, tadalafil and vardenafil in food supplements: A history, analytical aspects and health risks

“…It has already spread to another life-style drug (sibutramine) and might as well spread to essential drugs [100][101][102]. Proactive regulation of all possible analogues of registered ED drug substances may be useful.…”

Advanced Mass Spectrometry

“…Effect of thermal processing [66] LC-TOF Analysis of pesticides in fruits and vegetables [67] GC-TOF Quantitative analysis of acetaldehyde in foods consumed [68] LC-TOF Screening natural antioxidants in peanut shell [69] UHPLC-TOF Hexabromocyclododecane diastereomers [70] Type Application References UHPLC-TOF 19 antibiotics in dairy products [71] MALDI-TOF Microscale strategy to detect spermine and spermidine in food [72] LC-TOF Determination of phthalates in edible salts from food markets in Korea [73] LC-QqTOF Simultaneous determination five major antioxidant compounds [74] MALDI-TOF Monitoring of she-donkey's milk contamination or adulteration [75] MALDI-TOF Quantitating curcumin in food condiments and dietary supplements and screening of acrylamide-induced ROS protein indicators [76] LC-QqTOF Quantitating curcumin in food condiments and dietary supplements and screening of acrylamide-induced ROS protein indicators [45] UHPLC-TOF Analysis of illicit dietary supplements sold in the Italian market: Identification of a sildenafil thioderivative as adulterant [46] LC-TOF Simultaneous investigation of sesquiterpenes, pyrrolizidine alkaloids, and N-oxides in butterbur (Petasites hybridus) [77] UHPLC-QqTOF Determination of 141 pesticides in tea [78] UHPLC-QqTOF Determination of tadalafil and N-desmethylsibutramine in health and dietary supplements [79] LC-QqTOF Seven fluorescent whitening agents in food contact paper package materials [80] Lipidomics GC × GC-TOF Unsaponifiable fraction of lipids belonging to various types of milk [22] UHPLC-QqTOF Rapid and highly accurate detection of steryl glycoside [81] MALDI-TOF Rapid lipid profiling of bacteria [82] MALDI-TOF Detection of glycated phospholipids in heattreated food samples [83] …”

Scientific and Regulatory Perspectives in Herbal and Dietary Supplement Associated Hepatotoxicity in the United States

“…An important category of liver injury caused by exposure to both herbal and non-herbal preparations is hepatotoxicity caused by an adulterant(s) [ 72 , 119 , 120 , 121 , 122 , 123 , 124 , 125 , 126 , 127 , 128 , 129 , 130 , 131 , 132 , 133 , 134 ]. Adulterants that should not be present in dietary supplements may be introduced intentionally or unintentionally into the supply chain at any step between the planting phase and production and packaging phase of the marketed formulation.…”