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A rapid and sensitive method for the confirmation and quantification of sports performance pharmaceutical adulterants in dietary supplements using high-performance liquid chromatography coupled to tandem mass spectrometry was developed and validated. The  method presented here is applicable to the determination of  21 sports performance pharmaceutical adulterants. The sample preparation includes a methanol extraction and a dilution step. Chromatographic separation was performed on an InfinityLab Poroshell 120 Chiral-V column. The method was validated and proved to be linear, accurate, robust, and precise over the range 20 to 400 ng/ml (5µg/g to 100µg/g)  and with the detection limit of 2 µg/g for all compounds in different types of dietary supplements.  

2025 AOAC INTERNATIONAL Annual Meeting &amp; Exposition

Determination of Sports Performance Pharmaceutical Adulterants in Dietary Supplements by LC-MS/MS

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2025 AOAC INTERNATIONAL Annual Meeting & Exposition

The AOAC Annual Meeting & Exposition provides unparalleled professional development, networking, and collaboration in methods-based science.

Taraxacum kok-saghyz (TKS) is a sustainable industrial crop traditionally cultivated for natural rubber production. However, its pharmaceutical potential remains underexplored. In this study, we present an integrated green analytical platform to simultaneously recover natural rubber and pharmacologically active secondary metabolites from TKS roots and leaves. Using UPLC-MS/MS, we identified 1,813 metabolites, including caffeoylquinic acids, flavonoids, and lipid derivatives. Multivariate analyses (PCA, OPLS-DA) confirmed tissue-specific metabolic specialization, revealing 964 differentially expressed compounds between roots and leaves. Notably, leaf tissues were enriched in cynarin, chicoric acid, and luteolin derivatives—compounds known for antioxidant, hepatoprotective, and neuroprotective effects.
We implemented an ethanol–aqueous biphasic extraction to optimize compound preservation and co-extraction efficiency, validated via KEGG pathway mapping and mass spectrometric quantification. KEGG enrichment highlighted active biosynthesis of flavonoids and amino acid metabolites, supporting the nutraceutical relevance of TKS leaves. Root-specific enrichment of quinones and alkaloids suggests stress adaptation and antimicrobial potential.
This study demonstrates the feasibility of developing a dual-use biomanufacturing platform for botanical APIs and clean latex from U.S.-grown TKS. It contributes to the standardization of metabolite recovery from non-model plants and supports domestic sourcing of high-value nutraceutical ingredients. Our green extraction methodology enhances reproducibility and analytical rigor in dietary supplement development.

Integrated Extraction of Botanical Actives and Natural Rubber from Taraxacum kok-saghyz Using Green Analytical Techniques

Mycotoxins are naturally occurring toxins formed by fungi and have been shown to cause a variety of human health effects. Recent studies have shown that mycotoxins are occurring in areas of the world that historically have not had contamination, such as Aflatoxin in European wheat, presumably due to climate change. In this study, a method was developed using a high-end LC-MS/MS system to quantify multiple mycotoxins in cereals and food products at lower limits of detection. This is important because mycotoxin regulations have been lowered in some countries and regions. In addition, novel mycotoxins not routinely monitored have emerged, necessitating the expansion of the analyte panel. The method was applied to the analysis of various globally sourced toddler snacks.Preliminary data from the analysis of 30 toddler food samples showed that 94% were positive for at least one mycotoxin. Most of the samples contained mycotoxins from the Enniatin class with 47 positives found for this group. In addition, Beauvericin and the aflatoxins were also very prominent in the majority of the samples. The preliminary study was expanded to include toddler food samples from various regions around the world. These global trends will be presented as well as the results from various cereal grains.
 
 

Multi-Mycotoxin Analysis in Cereals and Toddler Food Using a High-End Triple Quadrupole Mass Spectrometer

Total ORAC 5 (Oxygen Radical Absorbance Capacity) is a series of five test methods that are used for the individual measurement of 5 different antioxidant capacities against its respective radical in functional ingredients and foods. These radicals are hydroxyl, peroxyl, peroxynitrite, singlet oxygen (1O2), and superoxide anion (O2-). Each of these test methods works on the principle of a fluorescent probe’s fluorescence being either oxidized or reduced by an active free radical species that was not inhibited by an antioxidant. The analysis takes place in a 96 well plate with various reference standards used and the final results being reported as umol Trolox equivalents per gram of material (umol TE/g) . These reactions are mixed, incubated, monitored and recorded using a fluorescence platereader. The degree of which the probe fluoresces is used to indicate the antioxidant capacity of the material. Each of the five antioxidant capacity test methods were individually validated and then combined into a single standard operating procedure and referred to as Total ORAC 5. The five methods can be referred to as ORAC (Hydrophilic Oxygen Radical Absorbance Capacity), HORAC (Hydroxyl Radical Absorbance Capacity, NORAC (Peroxynitrite Scavenging Activity Assay), SORAC (Singlet Oxygen Scavenging Activity Assay) and SOAC (Superoxide Scavenging Activity Assay). The validation incorporated method linearity/range, precision, accuracy, ruggedness, robustness and LOD/LOQ to demonstrate the method is fit for purpose.

A Method Validation for the Quantitative Analysis of the Antioxidant Capacity in Functional Ingredients and Foods by Total ORAC 5

Tang Kuei (Angelica sinensis) shares similar phytochemical profiles with other Angelica species, including A. archangelica, A. dahurica, A. decursiva, and A. acutiloba. These similarities—comprising volatile oils, polysaccharides, organic acids, and flavonoids—pose challenges for species identification using conventional methods like HPLC and HPTLC, especially in the absence of sufficient reference standards. To overcome these limitations, Ultra-Performance Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (UPLC-Q-TOF-MS) was employed, leveraging its high-resolution accurate mass (HRAM) capabilities to detect subtle differences in component profiles. Chromatograms of the test samples were compared with a botanical reference material (BRM) of A. sinensis, revealing two distinct peaks absent in the BRM. UPLC-Q-TOF-MS analysis identified the two peaks as decursin and its isomer, which are known markers predominantly associated with A. decursiva or specific subspecies of A. sinensis. This method integrates database searches with authenticated reference standards, allowing for precise identification of unknown compounds and confirmation of their botanical origins. It establishes a reliable framework for detecting deviations from the typical chemical profile of A. sinensis, effectively identifying potential contamination or adulteration by other Angelica species.

Identification of Angelica sinensis and differentiation of A. sinensis from other close species from Angelica Species Using UPLC-Q-TOF-MS

Most mycotoxins are chemically stable and survive food processing. Several hundred different mycotoxins have been identified, but the most observed mycotoxins that present a concern to human health and livestock include aflatoxins, ochratoxin A, patulin, fumonisins, zearalenone and nivalenol/deoxynivalenol. Most current reference methods for mycotoxin analysis still rely on non-confirmatory techniques such as TLC, HPLC-UV, and HPLC-FLD, with IAC cleanup often used to improve specificity. Regulatory bodies have only recently emphasized the need for standardized LC-MS methods, prompting the CEN to develop European standards under the M/520 mandate. Mycotoxins are typically extracted using liquid–liquid extraction for liquids (milk, wine, juices) and solid–liquid extraction for solids (cereals, dried fruits, spices), often with acidic buffers to enhance efficiency. The procedure enables the quantitative LC-MS/MS determination of regulated mycotoxins. Mass spectrometric parameters were optimized using Shimadzu’s Lab Solutions Connect software and get the best sensitivity, selectivity, and precision. This study presents a simple, high-throughput method for the determination of multiple mycotoxins in animal feed using the Shimadzu LCMS-8050RX system. Key steps included precursor ion selection and MRM optimization at different collision energies (CE), leading to a segmented MRM method with gradient elution. The mobile phase and column conditions were optimized using a GIST Shim-pack C18 AQ column to achieve better separation and peak shape. A commercially available animal feed sample was extracted, and a matrix blank was spiked with a standard mycotoxin mixture. The matrix-matched calibration curve ranged from 0.5 to 50 ppb, with accuracy between 80–120%. Spiked sample recoveries at 5 and 10 ppb were within 70–120%, in compliance with SANTE guidelines.

Quantitation of Multi-Mycotoxins in Animal Feed by Using Ultra-Fast LCMSMS

Herbal skincare (Ayurveda) products (HSPs) are used daily by many people around the world. Quality control of these products is immensely important to consumer safety, as the botanical ingredients used in HSPs are at risk of containing heavy metals (HMs) that can have adverse health effects. The Ministry of Ayush in India regulates HM levels in raw material (RM) and finished goods (FG). Given the wide range of fatty matter (0–100%) in HSPs, this study aimed to set up a robust method to quantitate HMs (As, Cd, Pb Hg, Sb, and Ni) in RM and FGs using Inductively Coupled Plasma Mass Spectrometry (ICP-MS), with tailored digestion programs for low and high-fat matrices.  Limit of detection (LOD) was determined by analyzing 20 reagent blanks resulting as 0.014 mg/kg for Hg and 0.001 to 0.067 mg/kg for other analytes. Limit of quantification (LOQ) for Hg, Ni, and other analytes was found to be 0.050, 0.203 and 0.100 mg/kg respectively. Repeatability (% RSDr) and reproducibility (%RSDR) at LOQ was established by analyzing six spike samples, resulting in 0.8879% to 13.35% and 1.66% to 19.69% respectively. Accuracy was demonstrated by spiking at 1x, 3x and 5x LOQ, and results ranged from 82.73% and 104.32% for RM and 81.75% to 125.85% for FG. This study emphasizes the need for rigorous quality control and regulatory monitoring in the HSPs industry to minimize consumer exposure to HMs and promote the development of safer and compliant products.

Simultaneous estimation of arsenic (As), cadmium (Cd), lead (Pb), mercury (Hg), antimony (Sb) and nickel (Ni) in herbal skincare products using ICP-MS

This study aims to the optimization of High-Performance Liquid Chromatography (HPLC) conditions for the separation of distinct peaks in a complex mixture using Design of Experiments (DOE) strategy. The objective was to evaluate and improve the resolution between Quercetin and Luteolin peaks by considering factors such as mobile phase composition, flow rate and column temperature. The design was employed systematically to study the impact of these variables on separation efficiency. The interaction effects of the factors were analyzed to determine the optimal conditions that would minimize peak overlap and enhance resolution. The results demonstrated the effectiveness of the DOE approach in identifying the critical factors influencing peak separation and provided insights into the optimal HPLC conditions for achieving distinct, well-resolved peaks. The approach also highlighted the importance of method and data analysis in optimizing HPLC method for complex sample analysis.

Optimization of HPLC Conditions for Improved Peak Separation of Quercetin and Luteolin Using Design of Experiments Approach

The functional mushroom industry represents a rapidly growing sector of agriculture with product offerings encompassing a wide variety of foods and dietary supplements.  The cultivation of numerous fungal species to provide sources of nutrition as well as promote health-related outcomes has been instrumental in driving this expansion.  One such species is Hericium erinaceus, whose mycelium has been extensively studied in preclinical assessments for its neuroactive effects.   This study involved a metabolomic characterization of solid substrate fermentation of brown rice by the prized gourmet and medicinal fungus, Hericium erinaceus (i.e. “lion’s mane,” “yamabushitake”, “hóutóugū”) over a four-week period. Samples were collected at 0, 7, 14, 21, and 28 days post inoculation and included 0- and 29-day uninoculated rice controls. We produced hydroethanolic and methanolic ethyl acetate extracts of the samples, which were then analyzed by Thermo Scientific Orbitrap Exploris 240 and Agilent 1260 Infinity II HPLC-DAD instrumental platforms.  Our findings indicate an apparent near-complete consumption of rice-derived lysolecithins by the fungus. Concomitantly, the biosynthetic production of a diverse range of bioactive fungal lipids over the course of the time series was observed.  Combined mass spectral and diode array detection datasets highlight specific grain-derived lipids as targets of fungal fermentation and clearly represent a chemically transformed substrate over time yielding known bioactive fungal metabolites of research interest.

Metabolomic Analysis of the Biotransformation of Lipids by Hericium erinaceus Mycelium through Fermentation of Brown Rice

Methane production by ruminant livestock is considered one of the major environmental concerns in the industry, and an increasing number of options, particularly feed additives, have emerged to mitigate methane emissions. The inclusion of bromoform in methane-reducing feed additives has rapidly evolved over the last few years. The need to accurately and precisely quantify bromoform in a wide variety of matrix types is crucial in order to ensure such additives are being used safely and effectively. To address these needs, several methodologies have been optimized and validated for the quantification of bromoform in various solid and liquid matrixes. Feed product samples, which contain higher concentrations of bromoform and can include Asparagopsis spp. or other bromoform-containing algae material, were methanol extracted utilizing a bead-beating approach. Animal product samples, blood, meat tissue and organs, and contain trace-level bromoform concentrations, followed a similar extraction process with hexane. Liquid samples such as milk or urine can be analyzed by an automated purge and trap system, similar to that already established in EPA 524.4. All extracted materials are analyzed by gas chromatography-mass spectrometry. These thoroughly tested methods and resulting validation data could become the basis of standardized regulatory protocols and therefore provide laboratories with a reliable, cost-effective, and easy to implement suite of analysis guidelines and procedures.

Quantifying bromoform in feed additives, livestock and food products using robust, validated, and standardized methods.

The AOAC Dietary Fiber & Other Carbohydrates (DFC) Program was established to address emerging challenges and evolving needs in the analysis of dietary fiber and other carbohydrates. To guide the program’s direction, an Advisory Panel comprising 14 representatives from participating organizations was convened to identify key priorities in this field. Based on their recommendations, the program’s initial project focused on developing a guidance document to assist stakeholders in selecting appropriate analytical methods for dietary fiber determination.
A dedicated working group—representing experts from over 21 countries and diverse sectors—was formed to lead this initiative. This group has developed a preliminary decision tree, presented here as a foundational draft. The draft is intended to serve as a framework for a comprehensive guidance document, shaped by input from the broader dietary fiber testing community. The ultimate objective is to deliver a practical, consensus-based tool that reflects global scientific expertise and supports consistent, accurate method selection for a wide range of sample types.

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