This research investigated the concentrations and dietary exposure of ochratoxin A (OTA) and zearalenone (ZEN) in edible vegetable oils among the Korean population. In 2022, 80 edible vegetable oil samples were collected from various retail sources in Korea. OTA was detected in 7.5% of the samples, and ZEN was detected in 62.5%. Dietary intake estimates were based on our findings and food consumption data from the Korean National Health and Nutrition Examination Survey. Dietary exposure was evaluated under lower bound, middle bound, and upper bound scenarios. The margin of exposure for OTA at the 95th percentile exposure exceeded 10,000 in all scenarios, indicating a low health concern. The estimated daily intake of ZEN under the three scenarios accounted for 0.03-0.11% of the tolerable daily intake of 0.4 μg/kg bw/day in the overall population, with the 95th percentile exposure reaching 0.11%, indicating that ZEN exposure from edible vegetable oils was well below the health-based guidance value. These results indicate that dietary exposure to OTA and ZEN from edible vegetable oils is not considered to pose a significant health risk to the Korean population.
Peanuts are among the most clinically important food allergens and may cause severe reactions even at very low exposure levels. This study investigated the presence of peanut residues in packaged baby biscuits marketed on the European side of Istanbul without peanut-containing ingredient declarations. A total of 100 packaged baby biscuit samples labelled as not containing peanut ingredients were collected from retail outlets in Basaksehir (n = 35), Eyup (n = 33), and Avcılar (n = 32) between January and June 2022 and analysed using a commercial ELISA kit (RIDASCREEN® FAST Peanut; analytical range 3.3-20 mg/kg, with a limit of detection of 3.3 mg/kg). The products consisted of plain, whole grain, goat's milk-based, vegetable-based, butter-based, apple-flavoured, and gluten-free baby biscuits. Peanut residues above the kit threshold (3.30 mg/kg) were detected in 15 samples (15%), with quantified values ranging from 3.94 to 4.93 mg/kg, while the remaining 85 samples (85%) were below the detection limit. No statistically significant association was found between product type and the presence of peanut residues. These findings demonstrate a potential risk of unintentional peanut presence in baby biscuits and highlight the need for strengthened allergen management, validated cleaning procedures, and accurate allergen labelling to protect sensitive consumer groups, particularly infants and young children.
The EU ban on the use of titanium dioxide (TiO2) as a food additive (E 171) has highlighted the need for harmonised and robust analytical methods to ensure uniform regulatory compliance and safeguard consumer health. This study compares three instrumental methods, namely portable X-ray fluorescence (pXRF), macro-Raman spectroscopy (applied to both intact and digested samples), and inductively coupled plasma mass spectrometry (ICP-MS), for detecting and quantifying titanium (Ti) or titanium dioxide (TiO2) in 35 chewing-gum samples of different shapes and colours, outlining their specific advantages and limitations. The results show that two items contained E 171, in agreement with the label declarations, and demonstrate, for the specific case of chewing gums where TiO2 is added to the coating, high concordance among the four applied analytical approaches. pXRF and Macro-Raman spectroscopy, when applied to intact samples, enable safe and rapid screening on the presence of Ti and TiO2 respectively in the sample's surface while a mild acidic digestion step followed by Raman analysis provides a confirmatory step for complex or interfered spectra. ICP-MS, despite relying on careful and laborious sample preparation, allows accurate quantitative results of Ti to estimate TiO2. Thanks to its sensitivity and elemental specificity, low Ti levels can be determined which however may not necessarily indicate intentional E 171 addition.
Acrylamide and 4-methylimidazole (4-MEI) are heat-induced contaminants formed during coffee roasting, raising concerns due to their potential toxicological effects. Considering the limited information about the occurrence of these contaminants in Brazilian coffees as well as the lack of studies on the effect of L-asparaginase treatment on both acrylamide and 4-MEI, this study evaluated (i) acrylamide and 4-MEI levels in 48 commercial roasted ground coffees sold in Campinas, Brazil, and (ii) the effect of L-asparaginase treatment on green Coffea arabica beans prior to roasting. Commercial samples were classified by coffee type (traditional, gourmet, organic, decaffeinated) and roast degree. For enzymatic treatment, three batches of green beans were treated (including steam) with Acrylaway® L at 5000 ASNU/kg, followed by roasting under controlled conditions. Acrylamide and 4-MEI were quantified by UHPLC-MS/MS and GC-MS, respectively; asparagine and ammonia precursors were measured enzymatically. Moisture content was monitored to ensure roasting consistency. Acrylamide concentrations in commercial coffees varied widely (from < LOD to 207.3 µg/kg) (LOD = 10 µg/kg), with traditional and light roast samples showing the highest levels (p < 0.05). In contrast, 4-MEI was strongly associated with darker roasts and ranged from < LOD to 366.1 µg/kg (LOD = 20 µg/kg). Packaging type had no significant effect on the concentrations of the contaminants. L-asparaginase treatment reduced asparagine by 23.8-34.1%, resulting in acrylamide reduction of 30.4-41.4% in roasted beans. Notably, 4-MEI levels remained unchanged after roasting, indicating that asparagine removal does not affect Maillard-derived imidazole formation pathways. Overall, combining steam pre-treatment with L-asparaginase effectively reduced acrylamide without promoting 4-MEI formation, demonstrating a viable mitigation strategy to enhance the chemical safety of C. arabica coffee while preserving roasting characteristics.
Thyrostats increase water retention and absorption in animals; this property is abused in the rearing of meat producing animals to inflate carcase weight in a bid to increase the profits of producers. As such meat is of poor quality, and due to the potential carcinogenic and teratogenic properties of thyrostats, their use has been banned in the EU since 1981. The difficulties encountered in the analysis of these compounds, due to their small size, high polarity, and the endogenous nature of some analytes (2-thiouracil, 4-thiouracil, 5-methylthiouracil), has limited the sensitivity of methods in difficult matrices such as urine, with minimum method performance requirements (MMPR) of 10 µg L-1 for six analytes (2-thiouracil, 5-methylthiouracil, propylthiouracil, tapazole/methimazole, benzylthiouracil and mercaptobenzimidazole). This work describes the development and alternative factorial validation, to the criteria as set out in CIR (EU) 2021/808, of a rapid and sensitive method for the quantitative confirmation of 11 thyrostats, including the endogenous analytes, using an extracted solvent standard calibration curve and post column infusion of NH4F, with decision limit (CCα) values ranging from 0.29 to 0.51 µg L-1.
Undeclared antibiotics in poultry feed contribute to exposure to antimicrobial drug residues, particularly in low- and middle-income countries where routine surveillance is limited by cost and laboratory constraints. Conventional analytical screening requires specialised equipment, making rapid, accessible alternatives valuable. This study evaluated the feasibility of re-purposing qualitative antibiotic screening techniques, originally developed and validated for milk, in rapid, multi-residue antibiotic detection in broiler feed after specialised sample pre-treatment. A microbial inhibition assay and three lateral-flow tests were validated through CCβ determination, stability assessment, and false-positive evaluation. Blank feed samples (pellets, mash, and crumbles) from three Belgian suppliers were spiked using milk detection limits, and 124 Kenyan commercial broiler feed samples (November - December 2022) were screened. CCβ values were established for twelve antibiotic classes. The inhibition assay offered broad detection but higher CCβ values (200 to > 100,000 µg/kg) than rapid tests (3-800 µg/kg). Rapid tests produced no false positives; the inhibition assay had one false positive in 30 samples (3.3%). Extracted samples remained stable for 24 h at 4 ± 2 °C, and frozen controls performed consistently. LC-MS/MS confirmed tylosin, quinolones, and five sulphonamides in 12 of 124 field samples. These methods, currently validated for use in milk, reliably detected multiple antibiotic classes in broiler feed, showing promise as practical monitoring tools for antibiotic contamination or carryover in feed in resource-limited settings.
Green coffee bean extract (GCBE) supplements are widely marketed for weight management, primarily due to their chlorogenic acids (CGAs) and caffeine content. This study evaluated the authenticity and quality of 23 commercial GCBE products by quantifying three major CGA isomers (3-CQA, 4-CQA and 5-CQA) and caffeine using HPLC-DAD. The CGA content ranged from non-detectable to 31.15%, with 5-CQA being predominant. Caffeine levels varied from non-detectable to 3.82%. Notably, two samples labelled as containing 50% CGAs had none detected, while several 'decaffeinated' products exceeded regulatory caffeine thresholds. Only three samples declared caffeine levels, none of which were fully compliant with their labels. Hierarchical cluster analysis (HCA) grouped the supplements into four distinct clusters based on total CGA and caffeine content, revealing widespread inconsistencies. These findings raise concerns over mislabelling, regulatory non-compliance, and potential health risks, underscoring the urgent need for stricter quality control and accurate labelling in the dietary supplement industry.
Acrylamide is a food contaminant formed via the Maillard reaction that may impair cardiometabolic health. Considering its role in oxidative stress, lipid peroxidation, and adipogenesis, acrylamide may compromise lipid and glucose profiles. The present study aims to assess acrylamide dietary exposure and test longitudinal associations with cardiometabolic outcomes from childhood to adolescence. From G21-birth-cohort, 3138 participants with at least 2 consecutive follow-ups from 4 to 13 years of age were included. Acrylamide dietary exposure was estimated using 3-day food diaries and occurrence data of acrylamide in food. Children presented a higher dietary acrylamide exposure than adolescents. The median exposure was, respectively, 0.79 µg/kg/d at 4 years and 0.44 µg/kg/d at 13 years. Both children (MOE = 215) and adolescents (MOE = 386) exposure levels presented health concerns regarding neoplastic effects. Cross-sectional and longitudinally, acrylamide dietary exposure was positively associated with blood glucose, waist circumference, and fat mass percentage. A negative association was found between dietary acrylamide exposure and z-BMI and cholesterol. This variability suggests that the effects of dietary acrylamide exposure on cardiometabolic health are complex and multifactorial. It was not possible to conclude, without uncertainty, that dietary acrylamide exposure is responsible for abnormalities in cardiometabolic outcomes from childhood to adolescence.
Alternaria toxins-particularly alternariol (AOH), alternariol methyl ether (AME), and tenuazonic acid (TeA)-are among the most concerning mycotoxins frequently detected in tomato paste, posing potential health risks to both adults and children. This study provides the first comprehensive investigation in Egypt assessing dietary exposure and the toxicological implications of these toxins in tomato paste, employing a rapid and streamlined analytical approach. The proposed method involves a 10 min sample preparation step followed by LC-ESI-MS/MS analysis with a 6 min run time. Method validation demonstrated robust analytical performance, with recovery rates ranging from 82% to 114%. Repeatability and intermediate precision (RSDs) ranged from 2.8% to 10.9% and 3.0% to 11.0%, respectively. Limits of detection (LOD) and quantification (LOQ) were in the ranges of 0.15-5 µg/kg and 0.5-20 µg/kg, respectively. Excellent linearity was achieved (R2 = 0.9999). The validated method was applied to 200 tomato paste samples collected across Egypt. The results revealed a widespread occurrence of AOH, AME, and TeA, with AOH identified as the predominant toxin, followed by AME and TeA. Although the estimated dietary intake (EDI) and the 95th percentile exposure levels for AOH and AME exceeded the threshold of toxicological concern, the calculated hazard quotient (HQ) values remained below unity, indicating no immediate health risk under current consumption patterns. Nevertheless, potential concerns remain for AOH and AME, particularly among high consumers and children. These findings provide a scientific basis for future mitigation strategies and further research aimed at reducing Alternaria toxin contamination in tomato paste.
Fresh vegetables, widely consumed agricultural products, have attracted considerable attention in food safety research, particularly on chemical contamination. Because vegetable-related risks are shaped by multiple interacting factors, this study develops a comprehensive risk evaluation index system and an associated composite calculation method for assessing food safety risks from chemical contamination in fresh vegetables. The Modified Delphi method was used to identify indicators at all levels. The analytic hierarchy process (AHP) was then applied to determine indicator weights, and an index calculation method was developed based on the comprehensive index method and the multiplicative synthesis method. Finally, this method was used to assess the risks of fresh vegetables in Guangzhou from 2017 to 2024. The final system comprises 5 primary indicators and 17 secondary indicators, and its scientific validity and reliability were confirmed. The empirical analysis showed that overall risk remained low over 2017-2024, and the total risk index was on an upward trend from 2017 to 2020, peaking in 2020. Among chemical categories, metallic elements, organophosphates and pyrethroids were the major contributors to total risk. Regarding vegetable varieties, leafy vegetables and fresh beans showed higher composite risk indices. The food safety risk index evaluation system developed in this study is scientifically grounded, feasible, and can serve as an effective tool for assessing the edible safety of fresh vegetables while providing new insights for food safety analysis.
The incorporation of zinc oxide nanoparticles (ZnO NPs) into biopolymers has gained attention for active food packaging due to their antimicrobial properties. However, potential Zn migration associated with safety concerns remains underexplored, particularly in non-regulated bio-based polymers. In this study, Zn migration from nanocellulose (NC) films incorporating spherical-, flower- and sheet-shaped ZnO NPs was evaluated, in ionic and nanoparticulate forms. Migration tests were conducted using water and ethanol 10% as food simulants under different time-temperature conditions. Zinc release was quantified using complementary analytical and microscopic approaches, and Fick's second law and Weibull models were employed to describe the migration kinetics. Migration behaviour was influenced by nanoparticle morphology, simulant type, and temperature. Zinc migrated predominantly as Zn2+, with minimal nanoparticle contribution, although distinction from cellulose fibres proved challenging. NC films containing flower-shaped nanoparticles exhibited the highest Zn migration, yet migration levels for all films remained below the European specific migration limit. Water promoted higher migration than ethanol, and unexpectedly, Zn migration was lower at 60 °C compared to 23 °C, likely due to matrix effect. Fickian fits yielded diffusion coefficients in the range 10-16-10-15 m2 s-1, while Weibull β < 1, confirmed diffusion-controlled release. These findings confirm the potential of NC/ZnO nanocomposites for food packaging applications and highlight the importance of combining multi analytics with kinetic modelling to support safety assessment.
Sugars may be added to coconut water to enhance sweetness or mask product dilution, necessitating the development of reliable methods for detecting such adulteration. This study evaluated proton nuclear magnetic resonance (1H NMR) spectroscopy combined with chemometric approaches to detect coconut water adulterated with high-fructose corn syrup (HFCS), cane syrup, glucose, fructose, and sucrose. A total of 120 authentic fresh coconut water samples and 150 adulterated samples (5-50% v/v, using sugar solutions adjusted to 5.1°Brix) were analysed. The one-class approach using data-driven soft independent modelling of class analogy (DD-SIMCA) showed strong capability to identify samples belonging to the authentic class, with 23 out of 24 authentic samples correctly identified (sensitivity = 0.958). However, specificity for rejecting adulterated samples was lower (0.700), with 45 out of 150 adulterated samples incorrectly accepted as authentic, resulting in an overall efficiency of 0.819. For binary discrimination, support vector machine (SVM) outperformed partial least squares-discriminant analysis (PLS-DA), misclassifying only three samples in the prediction set (balanced accuracy = 0.946) compared with ten misclassifications for PLS-DA (balanced accuracy = 0.817). For multi-class discrimination of adulterated samples, both models performed well, with PLS-DA correctly classifying all samples (balanced accuracy = 1.00), likely due to distinct spectral profiles among sugar types. Overall, the results demonstrate that 1H NMR spectroscopy combined with chemometric approaches provides a rapid and promising method for detecting undeclared sugar addition in coconut water.
Analysing plant-based food supplements is particularly challenging due to their complex composition. The inclusion of multiple plant species in a single product often results in overlapping or interfering signals when conventional chromatographic methods are used. To overcome these limitations, a novel approach was applied, integrating chromatographic fingerprinting with chemometric analysis and employing a multi-wavelength detection strategy to improve resolution and accuracy. Binary classification models were built to identify the presence or absence of regulated plant materials in the samples. These models achieved strong performance and were validated through both cross-validation and external test sets, ensuring the robustness of the results. A targeted market study of 25 samples arising from illegal sources was carried out, uncovering several noteworthy and concerning findings. This study focused on supplements marketed for potency enhancement, often linked to unregulated or illicit sources. The results revealed a significant occurrence of herbal adulteration, highlighting the urgent need for systematic screening protocols and stricter regulatory measures.
This study investigated acrylamide (AA) formation in dhal vade, a deep-fried snack made from yellow split peas, focusing on the influence of frying parameters and precursors. Using the Box-Behnken response surface methodology, the effects of frying time, temperature, asparagine, and glucose contents were evaluated. Frying time, temperature, and ASN significantly increased AA levels (p < 0.05), while glucose showed no significant effect (p = 0.20). The highest AA concentrations occurred at the maximum frying time and temperature. AA content showed a moderate negative correlation with moisture (r = -0.419), suggesting that rapid moisture loss enhances AA formation. Positive correlations were found with temperature (r = 0.768), time (r = 0.436), and weakly with ASN (r = 0.221) and glucose (r = 0.044). Pre-treatment of dhal with citric acid (CA) notably reduced AA by 40.7-58.6% in dhal vade and 20.6-33.1% in fried oil, depending on CA concentration (0.005 M and 0.01 M). AA content showed a moderate positive correlation with pH (0.482). The reduction may be attributed to CA-induced protonation of asparagine, delayed AA-forming reactions from water uptake, and leaching of precursors through tissue modification. Overall, optimising frying conditions and incorporating CA pre-treatment effectively minimise AA formation in dhal vade.
Ochratoxin A (OTA) is a mycotoxin of major concern in grape-derived products; however, information on its occurrence in fresh grape must remain limited. This study aimed to evaluate and adapt a high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method recommended by the International Organisation of Vine and Wine, originally validated for wine and grape juices, for the determination of OTA in fresh grape musts obtained from Vitis labrusca cultivars grown in Southern Brazil. Must samples from Bordô, Concord, Niagara Rosada, and Isabel were collected and characterised in terms of °Brix, °Babo, and total titratable acidity to assess maturity-related physicochemical attributes. Adaptation was required only for sample clarification, whereas sequential filtration was employed to overcome the high turbidity and soluble solids that may interfere with analytical reliability. The adapted method showed excellent linearity (R2 ≥ 0.999), satisfactory recoveries (83.75-104.6%), and limits of detection and quantification of 0.02 and 0.07 µg/L, respectively, in agreement with the Brazilian regulations. Only trace OTA peaks were detected, with no association observed between mycotoxin occurrence and grape cultivar or physicochemical maturity parameters. Overall, the proposed sample preparation proved suitable for routine monitoring at the pre-fermentation stage, supporting the safety and quality assessment of grape-derived products.
The contamination of cereals by mycotoxins, particularly zearalenone (ZEN), represents a global challenge for food safety and animal health. Brazil's diverse natural ecosystems also constitute an important reservoir of microorganisms with potential for biological control. This study evaluated the capacity of native Brazilian yeasts to adsorb ZEN using an in vitro model simulating pH conditions of the swine digestive system. Thirty-four yeast strains isolated from Brazilian biomes were initially screened for adsorption at pH 5.0, using 10 mg of biomass and a fixed ZEN concentration of 2.5 µg/mL. The effects of biomass amount (10, 20, and 30 mg) and pH variation (3-7) were subsequently evaluated using strains with the highest adsorption capacity. Adsorption isotherms were constructed with 30 mg biomass at ZEN concentrations ranging from 0.5 to 30 µg/mL under pH 3 and 6, and fitted to Hill, Langmuir, and Freundlich models. Adsorption increased with increasing biomass. The Hill model showed the best fit (R2 > 0.98), indicating positive cooperativity (n > 1) at all pH values, although the highest maximum adsorption capacity was observed at pH 3. Overall, Helenozyma melibiosica exhibited the greatest ZEN adsorption, while other strains also showed satisfactory performance.
Aluminium oxide (Alox) has long been recommended for use as an additional cleanup step to remove naturally occurring long-chain biogenic n-alkanes that interfere with the quantification of mineral oil saturated hydrocarbons (MOSH). However, the retention mechanism of Alox remains insufficiently understood, and the extent of MOSH loss across carbon-chain ranges during Alox treatment has not been systematically quantified. This study is the first to systematically quantify MOSH losses during Alox clean-up in a chain-length-resolved manner, based on the analysis of 150 vegetable oil samples representing 12 different oil types. The results demonstrate that MOSH below C20 is not measurably affected, while losses for C20-C25 remain below 5%, with progressively increasing losses observed at higher carbon numbers. These findings address the gaps described in earlier literature regarding Alox's uncertain retention behaviour as a pre-treatment method to quantify MOSH in vegetable oil samples. Quantitative MOSH profiling was further used to support a population-level dietary exposure assessment, indicating low MOSH exposure and high margin-of-exposure (MOE) values for the Chinese population. Collectively, this work provides critical analytical evidence supporting the appropriate application of Alox in MOSH determination and illustrates the relevance of the occurrence data generated in this study for screening-level exposure assessment of MOSH from vegetable oils.
This study investigated the comparative effects of vacuum and modified atmosphere packaging (MAP; 70% CO2 + 30% N2) on the formation dynamics of seven volatile N-nitrosamines (N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosopyrrolidine (NPYR), N-nitrosopiperidine (NPIP), and N-nitrosodibutylamine (NDBA)) in sausages during 12 weeks of refrigerated storage (4 °C). Weekly Gas Chromatography-Mass Spectrometry (GC-MS) analysis combined with two-way variance analysis (ANOVA) revealed that storage duration significantly increased all target nitrosamine concentrations (p < .005). Beyond standard statistical evaluation, a kinetic modelling approach was employed to elucidate the distinct reaction mechanisms driven by packaging atmospheres. The results demonstrated that the packaging type fundamentally dictated the formation kinetics. Notably, NDMA followed an "Acidity Controlled Delayed Growth" model under MAP, exhibiting a critical lag phase of 2.1 weeks (tlag) before accumulation commenced, whereas it remained below detection limits in vacuum packages. Furthermore, NPYR exhibited "Exponential Acceleration" kinetics in MAP, contrasting with the "Rapid Equilibrium" behaviour observed for NDBA and NDEA under vacuum conditions. These models achieved high determination coefficients (R2 > 0.90), mathematically demonstrating that packaging atmospheres shift underlying reaction pathways-from rapid saturation in vacuum to acid-catalyzed exponential growth in MAP. These findings underscore the necessity of evaluating nitrosamine dynamics within specific packaging contexts to ensure the chemical safety of processed meat products.
Cachaça is a Brazilian beverage produced exclusively from sugarcane, with an alcohol content between 38% and 48% (v/v) at 20 °C. The Identity and Quality Parameters stipulated by the Ministry of Agriculture and Livestock control the quality of the beverage, limiting secondary compounds and contaminants. Possible sources of contamination by some secondary compounds include inadequate sugarcane trimming and the presence of plant impurities in the production of cachaça because they contain compounds that participate in the pathways for the formation of secondary compounds. The objective of this study was to analyse the physical-chemical profile of cachaças produced under different conditions of cutting the stalks of six varieties of sugarcane, and correlate the concentration of secondary compounds with the cutting conditions: tip, point and stalk, point and stalk and only the stalk. The physical-chemical analyses followed Ministry of Agriculture and Livestock standards, and no sample exceeded the limits for cachaça. Four samples were classified as spirits because of their alcohol content. Samples with the presence of the apical meristem (tops of sugarcane shoots) presented higher levels of higher alcohols, suggesting that the amino acids in this region influence the formation of these compounds. Principal Component Analysis and Hierarchical Clustering indicated that the sugarcane variety exerts a greater influence on the final quality of the beverage than the conditions for cutting the raw material.
The increasing consumption of dietary supplements for weight management raises concerns about the presence of undeclared pharmaceutical substances, particularly diuretics. These compounds are sometimes added illegally to accelerate water loss and provide misleading weight-loss effects, but their uncontrolled use may lead to dehydration, electrolyte imbalance, kidney impairment, and potential doping violations. In this work, we developed and validated a simple and sensitive gas chromatography-mass spectrometry method for the simultaneous determination in dietary supplements of 14 diuretics of which 10 are sulphonamides. The method was optimised using selected ion monitoring for screening and SCAN mode for confirmation. The method was validated based on the guidelines of the International Conference on Harmonisation (ICH). Detection limits ranged from 15.68 to 160.83 ng/g in solid matrices and from 3.31 to 21.69 ng/mL in liquid matrices. Average extraction efficiency rates were between 65% and 95%. Intra-day and inter-day RSDs precision were below 8%. Furthermore, intra-day and inter-day accuracy ranged from 79% to 110% and from 81% to 112%, respectively, for the solid matrix, whereas for the liquid matrix, it ranged from 83% to 112% and from 82% to 114%, respectively. The validated method was applied to ten dietary supplement samples (capsules, tablets, powders, and liquids) collected from the Tunisian market. None of the tested products contained the investigated diuretics. This method is reliable for routine screening of adulterated supplements, contributing to consumer safety and public health monitoring.
