Simultaneous Analysis of Sexual Stimulants and Anabolic Steroids as Adulterants in Dietary Supplements by High Performance Liquid Chromatography with Photodiode Array Detection

Abstract

Background: The illegal virtual market for food supplements facilitates fraud and adulteration. Worldwide concern for consumer safety is growing on the part regulatory agencies, healthcare professionals and consumers. Objective: This work aimed to evaluate the presence of sexual stimulants and anabolic steroids commonly used in the adulteration of dietary supplements through the development of a high performance liquid chromatography with photodiode array detection (HPLC-DAD) method for the identification and quantification of these compounds. Method: The mobile phase composed of an ammonium acetate solution, acetonitrile and methanol leaded to the efficient separation of vardenafil, testosterone base, testosterone propionate, tadalafil, sildenafil and yohimbine. Results: The assay was linear (r2> 0.999), precise (RSD% <0.5), accurate (99.1 to 105.2%), and the limits of detection and quantification were less than 0.05 and 0.15 μg/mL, respectively. Four samples of dietary supplements contained testosterone (n=1), tadalafil (n=2) and yohimbine (n=1) as adulterants. The adulterants found were in subtherapeutic doses, probably to reduce possible adverse effects and the action expected to appear natural. Since about 80% of adverse drug reactions are dose dependent. However, unpredictable adverse drug reactions are dose independent and based on idiosyncratic or allergic mechanisms or intolerance. Conclusion: The developed method is convenient and easily applicable for adulteration detection of the analyzed drugs in the multicomponent supplements.

Interpol Review of Drug Analysis 2019-2022

“…2019 Rapid detection of adulteration of dehydroepiandrosterone in slimming products by competitive indirect enzyme-linked immunosorbent assay and lateral flow immunochromatography [ 832 ]; screening method for detection of illegal adulterants in ginseng pills by profiling analysis of HPLC multi-dimensional fingerprints [ 833 ]; 2020 identification of tert-butyl-4-anilinopiperidine-1-carboxylate (4-anilinopiperdine-t-BOC or 4-AP-t-BOC) in seized falsified ‘Xanax’ tablets and suspected heroin seizures [ 834 ]; 20 herbal mixtures containing Cumyl-PEGACLONE were quantitatively analyzed by HPLC-DAD after an initial screening by gas chromatography mass spectrometry [ 835 ]; simultaneous and reliable determination of 20 pharmaceutical compounds in adulterated health food products using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) and liquid chromatography with quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) [ 836 ]; MALDI-MS method for analysis of illegal drugs and doped substances added in supplements [ 837 ]; 2021 voltammetric method for analyzing weight loss products adulterated amphetamine [ 838 ]; development and validation of an HPLC-MS/MS system for the analysis of 16 chemical drugs illegally added to dietary supplements for weight-loss in a capsule form [ 839 ]; quantification of pharmaceuticals or prescription medications (fluoxetine, phenolphthalein, and sibutramine illegally added to herbal weight loss supplements by RP-HPLC-MS/MS [ 840 ]; IMS qualitiative screening method for illicit additives (ibuprofen, nitrazepam, nitrendipine, indomethacin, phenobarbital, sibutramine, diclofenac sodium, diazepam, estazolam, melatonin, phenolphthalein, prednisone acetate, betamethasone, metformin HCl, glibenclamide, and tadalafil) in herbal pharmaceuticals and health foods with quantification by HPLC [ 841 ]; UPLC-PDA and LC/EIS-MS/MS methods for simultaneously screening for 25 anti-hyperlipidemic substances illegally added to dietary supplements [ 842 ]; HPLC-DAD method for the identification and quantification of sexual stimulants and anabolic steroids in the adulterated dietary supplements [ 843 ]; MALDI-MS method for the analysis of illegally added and doped substances added to medicines or food [ 837 ]; 2022 mixed-mode sorbent for SPE of hydrophobic and hydrophilic illegal additives from food sample followed by analysis by RPLC/HILIC-MS/MS [ 844 ]; analytical techniques and metrological principles in studying dietary supplement products and ingredients, particularly medicinal plants and other botanicals [ 845 ]; a membrane-protected micro-SPE method based on molecular imprinting and its application to the determination of local anesthetics illegally added to cosmetics [ 846 ]; application of predicted fragmentation pathways and fragment ion structures with LC-QTOF-MS for the analysis of 15 steroids and 20 selective androgen receptor modulators in dietary supplements [ 847 ]; development of an atmospheric pressure solids analysis probe coupled with single-quadrupole mass spectrometer (A...…”