Analytical Challenges and Metrological Approaches to Ensuring Dietary Supplement Quality: International Perspectives

Abstract

The increased utilization of metrology resources and expanded application of its’ approaches in the development of internationally agreed upon measurements can lay the basis for regulatory harmonization, support reproducible research, and advance scientific understanding, especially of dietary supplements and herbal medicines. Yet, metrology is often underappreciated and underutilized in dealing with the many challenges presented by these chemically complex preparations. This article discusses the utility of applying rigorous analytical techniques and adopting metrological principles more widely in studying dietary supplement products and ingredients, particularly medicinal plants and other botanicals. An assessment of current and emerging dietary supplement characterization methods is provided, including targeted and non-targeted techniques, as well as data analysis and evaluation approaches, with a focus on chemometrics, toxicity, dosage form performance, and data management. Quality assessment, statistical methods, and optimized methods for data management are also discussed. Case studies provide examples of applying metrological principles in thorough analytical characterization of supplement composition to clarify their health effects. A new frontier for metrology in dietary supplement science is described, including opportunities to improve methods for analysis and data management, development of relevant standards and good practices, and communication of these developments to researchers and analysts, as well as to regulatory and policy decision makers in the public and private sectors. The promotion of closer interactions between analytical, clinical, and pharmaceutical scientists who are involved in research and product development with metrologists who develop standards and methodological guidelines is critical to advance research on dietary supplement characterization and health effects.

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...…”

Detecting and Profiling of Milk Thistle Metabolites in Food Supplements: A Safety-Oriented Approach by Advanced Analytics

“…Nuclear magnetic resonance (NMR) spectroscopy is a non-destructive technique used in quality control and research to determine the content and the purity of a sample, as well as its molecular structure [ 123 ]. NMR-based untargeted metabolomic was proposed for the discrimination of authentic versus potentially adulterated botanicals [ 94 ].…”

“…Driven by the increased public demand, the research community, the regulatory authorities, and Pharmacopeias are making high contributions and proposing novel strategies for the identification and authentication of botanicals and their derived preparations in the context of the quality control [ 38 , 94 , 123 ]. The global regulatory agencies are advocating and supporting the use of orthogonal methods that are fit for purpose and can discriminate closely related species to ensure the quality and safety of herbal medicine and dietary supplements [ 33 ].…”

Acute Coronary Syndrome in the COVID-19 Era—Differences and Dilemmas Compared to the Pre-COVID-19 Era

“…Currently, the data are insufficient to support the recommendations for or against the use of any vitamin, mineral, herb or other botanical, fatty acid, or other dietary supplement ingredient for the prevention or treatment of COVID-19 [ 96 ]. Some authors suggest that the use of several dietary supplements, such as garlic, ginger, cranberries, oranges, omega-3 and -6 polyunsaturated fatty acids, vitamins (e.g., vitamins A, B vitamins, C, D, and E) and minerals (e.g., Cu, Fe, Mg, Mn, Na, Se, and Zn), have potential antiviral activity [ 97 ].…”