Food Additives and Contaminants Part A-chemistry Analysis Control Exposure & Risk Assessment最新文献

Deoxynivalenol (DON) contaminates various complex matrices, necessitating straightforward, effective cleanup and precise detection methods. This study employed immunomagnetic beads for sample purification and utilized a competitive time-resolved fluoro-immuno-chromatographic assay to achieve quantitative detection of DON in corn and its by-products. The limits of detection and quantification were 104 μg/kg and 243 μg/kg, respectively. Significant cross-reactivity was absent with most common toxins, except for 3-acetyl-deoxynivalenol, which exhibited a cross-reaction rate of 3167%. The recovery rates ranged from 86% to 117%, with coefficients of variation between 6.9% and 9.5%. The correlation coefficient with HPLC was 0.977. This method is rapid, accurate, and requires no large-scale equipment, facilitating on-site detection directly.

Plasma, milk and tissue samples were collected from 30 dairy cattle (0.4 to 8.9 years of age) with lifetime exposures to perfluoroalkyl substances (PFAS) removed from a PFAS-contaminated farm and provided PFAS-free feed and water. Twenty cattle were slaughtered 2 weeks after removal from the farm and tissues were collected for histological and residue analyses. Milk and/or plasma were collected from all remaining cattle at 2-week intervals and milk samples were collected daily but were analyzed at the same intervals as plasma samples. The remaining cattle were slaughtered 20 and 22 weeks after the initial set of 20 animals were slaughtered. While many incidental and normal background findings were noted on histological evaluation, no consistent histological finding was associated with PFAS exposure. Perfluoroalkyl carboxylic acids (PFCA) and perfluoro butane sulfonic acid (PFBS) were not generally detected in milk, plasma and tissues, but perfluoroalkyl sulfonic acids (PFSA) were quantifiable throughout the 22-week withdrawal period in most matrices. Estimated plasma half-lives of perfluorohexane sulfonic acid (PFHxS), perfluoroheptane sulfonic acid (PFHpS), linear perfluorooctane sulfonic acid (L-PFOS), perfluoro-3-methyl heptanesulfonate (3Me-PFOS) and perfluoro-6-methyl heptanesulfonate (6Me-PFOS) ranged from 4 to 10 weeks, but the estimates were associated with large confidence intervals. Across animal status (heifer, lactating, dry), natural log transformed (Ln) plasma residues of PFHxS and L-PFOS were generally well correlated with Ln-transformed PFHxS and L-PFOS residues in lung, muscle, liver and kidney (R², 0.7572 to 0.9394) whereas the strongest relationships of Ln-transformed L-PFOS residues among tissues were between lung and liver, kidney and muscle (R², 0.8287 to 0.9138).

Illegal additives such as oxyphenisatine and its esters are prevalent in the slimming food industry, necessitating a robust analytical method for their detection. This study presents a novel UPLC-MS/MS method for the rapid and accurate quantification of total oxyphenisatine levels in fermented green plum, following hydrolysis of its esters. An efficient ultrasonic extraction with a methanol and 0.1 mol/L NaOH mixture (5:5, v/v) was optimised to hydrolyse esters to oxyphenisatine within 18 min. Chromatographic separation was conducted on a C18 column (Waters Acquity UPLC BEH, 2.1 × 100 mm, 1.7 μm) with a mobile phase of 5 mmol/L ammonium acetate and acetonitrile under gradient elution at a flow rate of 0.3 mL/min. The method demonstrated linearity (r² > 0.999) over 0.1-500 µg/L, with a LOD of 10 µg/kg and LOQ of 30 µg/kg. Quantitative analysis employed positive ion multi-response monitoring and external standardisation, achieving recoveries of 92.4-97.0% and RSDs of 2.9-4.1%. Application to ten real samples gave a 90% detection rate, with measured values closely aligning with theoretical predictions (-11.3 to 13.2% relative difference) and oxyphenisatine content ranging from 159 µg/kg to 452 mg/kg. This UPLC-MS/MS method provides a reliable and efficient tool for monitoring the presence of oxyphenisatine and its derivatives in the context of food safety.

A competitive direct enzyme-linked immunosorbent assay (dc-ELISA) was developed for the detection and quantification of scopolamine (SCO) in wheat flours and cereal samples (multigrain, oat and barley). The limit of quantification (IC₂₀) of the established method was 6.00 ± 1.20 ng/g, with the limit of detection (IC₁₀) being 2.4 ± 0.6 ng/g in wheat flour with a coefficient of variation (CV) less than 20%. The assay was highly specific to SCO and nor-scopolamine, with no cross-reactivity to other similar structures. In spiked wheat flours the recoveries ranged from 84% to 104% with CVs of less than 20% and the recovery from a Food Analysis Performance Assessment Scheme (FAPAS) buckwheat control sample was 118%. A comparison of spiked wheat flour and a FAPAS control sample showed similar results to those determined by classical LC-MS/MS methods. A small retail survey of wheat flours and cereal samples was conducted using this ELISA method and a LC-MS/MS method, which showed scopolamine was not detected in any of these survey samples by either method. This method is suitable for rapid quantitation of SCO in wheat flours and cereal samples.

Beehives can accumulate environmental contaminants as bees gather pollen, propolis, and water from their surroundings, contaminating hive products like honey. Moreover, in multifloral environments, bees can interact with plants treated with different pesticides, often causing higher pesticides concentrations in multi-floral honey than in mono-floral varieties. Glyphosate and glufosinate are both widely used herbicides. Glyphosate accounted for one-third of herbicide sales in Europe in 2017 and continues to raise health concerns, including its potential carcinogenicity. While the European Commission extended glyphosate's authorisation for another 10 years in 2023, concerns remain about its impact on biodiversity and human health. This study aimed to monitor the presence of glyphosate, glufosinate, and their metabolites in 100 samples of multifloral honey representing Italian production by analysis using IC-HRMS. Results indicated that 12% of honey samples contained glyphosate residues ranging from > LOQ to 45 ng g^-1, with the highest concentrations detected in the Puglia region. No sample exceeded the maximum residue levels set by EU regulations. Glufosinate and its metabolites were not detected in any samples. These findings underscore the need for continued monitoring of pesticide residues in honey, particularly given the potential 'cocktail effect' of multiple contaminants and their combined toxicity. This study highlights the importance of safeguarding consumer health, especially in vulnerable populations, by addressing gaps in data on pesticide residue levels.

Two novel phosphodiesterase 5 (PDE-5) inhibitors were detected in pressed candy using high-performance liquid chromatography (HPLC)-diode array detection. Following extraction with acetonitrile and sonication, the compounds were isolated and purified via semi-preparative liquid chromatography. Structural characterisation was achieved through high-resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) spectroscopy. The results indicate that both compounds possess identical UV absorption spectra. The molecular formulas of compounds 1 and 2 are C₂₃H₃₂N₄O₄ and C₂₂H₃₀N₄O₄, respectively, each featuring a pyrimidinone benzene structure with a single methylene group (-CH₂) variation. As studies on these illicit compounds in functional foods have not been conducted, regulatory agencies must take note and incorporate them for the assessment of illicit additives in functional and healthcare foods.

This study covered the evaluation of performance characteristics and validation of five commercial ELISA kits for the detection of a banned antimicrobial, chloramphenicol (CAP), in muscle and aquaculture products. CAP has been banned in the European Union since 1994, but is still authorised in some countries in the world. In 2019, the European Union set a new Reference Point for Action (RPA), decreasing the acceptable limit of CAP in animal tissues for human consumption from 0.30 µg/kg to 0.15 µg/kg. Validations were performed according to the European Regulation EC/2021/808 and to the European Guideline on Screening Method Validation (2023). The detection capabilities CCβ were all determined under the RPA, but were 3 to 15 times higher than the announced limit of detection (LOD). False negative rates were satisfactory for all the kits (≤ 5%) and false positive rates were acceptable. All of them were found out to be applicable to aquaculture products and meat at a common CCβ.

Algae supplements are widely recognized for their nutritional benefits and are commonly marketed as natural health products. However, concerns regarding contamination with cyanobacterial toxins have been raised. Moreover, there is very little data regarding the potential contamination of algal supplements on the Chinese market by these toxins. In this study, we employed a validated solid-phase extraction ultra-high-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method to analyze algal supplements available in China. Therefore, this study optimized the extraction conditions for twelve microcystins (MCs) simultaneously using response surface methodology (RSM) and analyzed via UHPLC-MS/MS. Method validation was conducted in four supplement matrices (capsule, liquid, powder, and tablet) to ensure the method's accuracy, sensitivity, and reproducibility. Analysis of nineteen commercial algae products available in China using the validated method revealed the presence of four MCs: microcystin-LF (MC-LF), microcystin-LR (MC-LR), microcystin-LA (MC-LA), and microcystin-YR (MC-YR). Furthermore, seven products were found to contain one or more of the MCs, with two products exceeding the 1 μg/g MC limit. These findings underscore the effectiveness of the validated method in assessing MC contamination of algae supplements and consequently identifying consumers expected to be at risk from prolonged exposure to recommended daily algal supplements.

In this study, residue depletion and withdrawal time estimation of tilmicosin were examined in Taihe black-bone silky fowls (TBSFs) after oral administration for three consecutive days at a dose of 75 mg/L in water. The tilmicosin concentrations in liver, kidney, muscle, and skin/fat of TBSFs collected from different time points (0.16, 1, 3, 5, 7, 9, 12, 20, 30, 40 days after last administration) were determined by UPLC-MS/MS. The results indicated that the tilmicosin concentrations in TBSFs tissues varied significantly, and kidney had the highest average concentrations (2604.65 ± 4625.20 μg/kg), followed by liver (1125.54 ± 1479.24 μg/kg), skin/fat (372.81 ± 428.33 μg/kg), and muscle (104.52 ± 143.95 μg/kg). Meanwhile, tilmicosin was still detected in all the four studied tissues (liver, kidney, skin/fat, and muscle) of TBSFs at the last time point (40th day after administration), suggesting that tilmicosin in TBSFs depleted slowly. Based on our experiments, the recommended withdrawal time of tilmicosin for TBSFs after oral administration for three consecutive days at a dose of 75 mg/L in water should be 32 days, which is much longer than the duration specified by Chinese regulatory authorities (10 days), and the abundance of melanin in TBSFs might be responsible for this phenomenon. Hence, a special use and withdrawal procedure of veterinary drugs in TBSFs is needed, and it is essential to focus on potential involvement of melanin in tilmicosin accumulation.

Polyethylene terephthalate (PET) is one of the most commonly used packaging materials for beverages. The increased use of PET has contributed to the rise in plastic waste. Recycled PET (R-PET) is a solution to address this environmental issue. This study aims to determine the migration level of Pb, Cd, Hg, and Sb in PET bottles, evaluate the effect of plastic types (virgin PET and R-PET) and testing conditions (according to BPOM following national regulation and EU following international regulation) on the migration from heavy metals into food. Sixty test samples of virgin PET and R-PET bottles, obtained from four packaging industries in Indonesia, were analyzed for Cd, Hg, Pb, and Sb concentrations using ICP-MS. The results showed that the highest concentrations of heavy metal migration for Cd and Pb were in a virgin PET sample according to BPOM, respectively, at 28 ± 2 ng/L and 636 ± 22 ng/L. Meanwhile, the highest concentrations of Hg and Sb were in a R-PET sample according to EU, respectively, at 469 ± 91 ng/L and 5042 ± 617 ng/L. There was a significant difference in heavy metal levels between the two types of plastic (virgin PET and R-PET) and two testing conditions (BPOM and EU). However, all the obtained concentrations were below the permitted limits of national and EU regulations.