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

Green coffee beans, rejected for commercial use because of glyphosate contamination, were examined to monitor their glyphosate levels from harvest, through roasting, until various coffee extractions. The green beans, Arabica and Robusta, exhibited glyphosate levels above the EU-MRL (0.14-0.21 mg/kg), representing a worst-case scenario. The beans were roasted to different degrees and subsequently used for different coffee preparations. As a result of roasting (>200 °C), glyphosate contents were reduced, frequently by more than 73%. Remarkably, up to 9% of initial glyphosate was removed together with the silverskin, already at lower temperatures. Filtered and instant coffee beverages prepared from respective coffee samples resulted in virtually quantitative glyphosate transfer. Glyphosate transfer was significantly less for espresso, and ristretto, apparently due to the reduced amounts of water used for extraction. Aminomethylphosphonic acid (AMPA) was not detectable on any process level, confirming that AMPA is not a thermal glyphosate degradation product. In conclusion, compelling evidence is provided that glyphosate contamination becomes considerably reduced during roasting, whereas beverage preparation contributes at best to a minor further reduction. In consequence, even unusually high initial glyphosate loads in green beans are strongly reduced by the roasting process, resulting in a final cup content of <0.4 µg.

Tansy ragwort (Senecio jacobaea L.) growing in animal pasture may pose a risk to humans due to the potential transfer of pyrrolizidine alkaloids (PAs) into food of animal origin. Here, we investigated what amount of PAs corresponds to the amount of ragwort consumed by sheep on a pasture and whether the ingested PAs are transferred into edible tissue. From 2020 to 2021, a field study was conducted with 70 sheep grazing on a pasture (stocking density of 12 sheep/hectare) with considerable quantities of tansy ragwort. After slaughter, blood samples were taken for analysis of liver enzyme activities and haemoglobin concentration. Samples of ruminal fluid, liver and diaphragm pillar were analysed for PAs. The amount of ingested ragwort was determined by counting missing plant parts and calculating their weight using reference material. The mean daily intake of ragwort per sheep ranged from 0.16 kg to 4.89 kg fresh matter and corresponded to PA doses from 0.3 to 40.9 mg/kg body weight with no effect on the liver enzyme activities. The PA concentrations in the animal tissue were between the limit of detection and a maximum of 8.0 µg/kg in the liver and 2.5 µg/kg in muscle. These data suggest that the risk is negligible of exposure to PAs through consumption of meat or liver.

Carvacrol is a consolidated natural antimicrobial. However, its use in food is a challenge due to characteristic odour and high volatility. Nanoencapsulation has emerged to overcome these drawbacks. Aspergillus spp. represent a concern in grapes for causing rot and producing mycotoxins. This study aimed to evaluate the effect of carvacrol (unencapsulated and loaded into Eudragit^® and chia nanocapsules) on the growth of Aspergillus species. Spore germination and mycelial growth of Aspergillus spp. were evaluated using the agar dilution culture method. The stability of nanocapsules during storage was monitored monthly by evaluating the particle size distribution, polydispersity index, and zeta potential. Antifungal and antitoxigenic effectiveness of nanocapsules were assessed by counting fungal colony-forming units and determining mycotoxin levels in grapes. A dose-dependent effect of carvacrol (unencapsulated and encapsulated forms) on spore germination and mycelial growth was observed. During 180 days of storage, carvacrol into Eudragit^® nanocapsules preserved their nanometric dimensions, whereas chia nanocapsules maintained this characteristic for 30 days. The antifungal effectiveness of both encapsulated forms persisted for 210 days. No mycotoxin was found, even when fungal growth was not completely suppressed. Nanoencapsulated carvacrol proved to be a new promising antifungal product to ensure quality and safety in the grape production chain.

Miniaturized procedures for chemical analysis give the possibility of a significant reduction in quantities of organic solvents used during isolation and determination processes. Liquid-liquid microextraction (LLME) using butanol as an extractant was investigated to selectively isolate oxytetracycline (OTC) antibiotic residues from dairy products. The optimal conditions of LLME were established after deproteinization of the samples. The isolation procedure for OTC was performed using 700 µL of butanol. The extracts were analysed by HPLC-UV and LC-MS/MS. A satisfactory analyte recovery was achieved in the range 97.6%-98.9%. The concentration of the linearity range of the studied antibiotic should allow its determination at the level of MRL values. The limit of detection during HPLC-UV and LC-MS/MS determination of OTC in milk samples was 9.9·10^-8mol L^-1 (47.85 µg kg^-1) and 5.7·10^-9mol L^-1 (2.75 µg kg^-1), respectively. The precision (1.7%-8.6%) of the methods using LLME isolation of OTC varied depending on the kind of sample and the chromatographic technique used. The developed methods were applied to the analysis of milk and cottage cheese to estimate the presence and detection of OTC content.

Fluorotelomer-based acrylate polymers and surfactants used to grease-proof food contact paper (FCP) are potential sources of dietary exposure to perfluoroalkyl substances (PFAS). Food contact substances (FCS) containing polyfluorinated long-chains (≥C8) were voluntarily removed by their manufacturers from the U.S. market in 2011 due to health concerns and largely replaced with FCSs containing short-chain (≤C7) PFAS. In 2020, FDA findings of potential biopersistence of 6:2 FTOH (CF₃(CF₂)₅CH₂CH₂OH) similarly prompted an additional voluntarily phase-out of FCSs containing 6:2 FTOH by their manufacturers that was completed by the end of 2023. To monitor the phase-out process, a screening method was developed to detect FCPs containing ester-linked polyfluorinated pendant chains. Direct Analysis in Real Time-Isotope Dilution-High Resolution Mass Spectrometry (DART-ID-HRMS) enabled rapid semi-quantitative detection of 6:2 FTOH in FCP saponification reaction headspace without requiring sample concentration or chromatography. ¹⁹F-NMR analysis confirmed 6:2 FTOH pendant chain identity and detection dependence on saponification. The speed and specificity of this approach arise from ester saponification in the presence of stable isotopically labeled 6:2 FTOH; high FTOH differential volatility relative to nonfluorinated matrix, and the facile production of FTOH gas-phase anions (e.g., [M + O₂]^·-, [M-H + CO₂]^-) under ambient ionization conditions. The efficiency of this simple workflow makes it well-suited for monitoring the phase-out of FCS containing ester-linked polyfluorinated chains from the U.S. marketplace.

We evaluated the co-occurrence of arsenic (As), cadmium (Cd), and lead (Pb) in 10 categories of processed foods intended for infants and young children (<2 years old) and adapted methodology to characterise and evaluate the impact of correlations on toxic element (TE) concentrations in these foods. Co-occurrence was assessed by calculating the frequency of samples having concentrations above the limit of detection (LOD) among TE sets (i.e. As-Cd, As-Pb, Cd-Pb, and As-Cd-Pb). Pairwise correlations were evaluated using two statistical approaches adapted to censored data: (i) non-parametric Kendall's tau and (ii) parametric Bayesian modelling. Nonparametric and parametric correlation analyses showed similar results. We found positive correlations among one or more pairs of the TEs (As, Pb, and Cd) in 9 of the 10 categories of foods intended for infants and young children and a negative correlation for one TE pair for a single food category. Where positive correlations are observed, removing samples with high concentrations of a given TE reduces the mean of the other TEs in that food. We also explored the impact of correlations among TEs on the fraction of the supply below maximum levels. Positive correlations among TEs have the potential to reduce the impact on the supply when setting multiple maximum levels.

Analysis of bulk wheat consignments for naturally-occurring contaminants and residues from plant protection products is common, and helps manage potential health risks to consumers. The heterogeneous distribution of some mycotoxins in wheat has been described, however the distribution of other contaminants and residues has not yet been reported. This study characterized distributions of deoxynivalenol, ochratoxin A, ergot alkaloids, cadmium, and glyphosate in nine large consignments of wheat by analysing composite samples representing sub-lots prepared from increments obtained during the entire loading process. The widest span of concentrations within a consignment occurred for ochratoxin A (<0.5-22.9 µg/kg) and ergot alkaloids (0.009-0.486 mg/kg), followed by deoxynivalenol (<0.05-0.76 mg/kg) and glyphosate (<0.3-5.01 mg/kg), and then cadmium (0.022-0.102 mg/kg). Experimental semivariograms were plotted to model the spatio-temporal correlation of analytes within consignments during loading. Analyses demonstrated that distributions of contaminants and residues within a particular consignment differed, and that distributions of a particular contaminant or residue differed among consignments. The results indicate that sampling during only a portion of a loading or unloading process can result in a composite sample that is not representative of the consignment and thus increase the risk of misclassifying a consignment as compliant.

This study analyzed the residue depletion kinetics of ivermectin (IVM) in Nelore and crossbred (Nelore x Angus) cattle aiming to compare the profiles between the breeds and evaluate the residue levels at the injection site. IVM 1%, at a dose of 0.2 mg/kg, was administered via the subcutaneous route, and tissue samples were collected on different days post administration for analysis by LC-MS/MS. The results revealed that the detection of the marker residue in conventional matrices such as the liver, perirenal fat, and trapezius muscle (injection site) had relatively high residue concentrations. The maximum residue limit (MRL) was exceeded at the injection site at 21- and 35-days post administration in crossbred and Nelore animals, respectively, with significant variations between animals. This study highlighted significant challenges in accurately determining the pharmacokinetic profile and withdrawal periods of IVM in cattle due to high variability in tissue residue data, particularly at injection sites. The comparison of IVM concentrations between cattle breeds was hindered by high standard errors, emphasizing the need for more rigorous sampling protocols. The results suggest that current guidelines may not adequately account for the erratic depletion kinetics of injectable formulations like IVM, especially at injection sites. Therefore, improving sampling techniques and revising guidelines are essential for accurate residue monitoring and withdrawal period determination.

This study was conducted to monitor and evaluate the health risks of multiple organophosphorus pesticide residues in three characteristic fruits of Maragheh district, East Azerbaijan province. The Monte Carlo method was used to quantify the possible non-carcinogenic health risks associated with pesticide residues in adults and children. The residues of 17 pesticides in 36 samples were analysed using the QuEChERS extraction method coupled with gas chromatography-mass spectrometry (GC/MS). Residues of 13 pesticides (76.47%) were detected in grape samples and 15 pesticides (88.23%) in apricot and plum samples. The maximum level found in grape samples was due to chlorpyrifos with 1.2 mg/kg, and in apricot and plum samples to diazinon with 1.6 and 1.3 mg/kg, respectively. All grape, apricot and plum samples contained at least ten pesticides with levels exceeding the Iranian and EU Maximum Residue Limits (MRLs). The processing factor for washing treatment in grape, apricot and plum samples was less than 1, ranging from 0.53 to 0.69. Chlorpyrifos with values of 0.064 and 0.256 in the grape samples and diazinon with values of 0.0443 and 0.177 in the apricot samples and values of 0.0263 and 0.105 in the plum samples contain the highest hazard quotients (HQ) for adults and children, respectively. The cumulative risk assessment due to exposure to several pesticide residues suggests that there is no significant health risk for adults (HI < 1). However, consumption of unwashed grapes may cause adverse effects in children (HI = 1.48). However, for further research, a comprehensive longitudinal study is suggested to assess the long-term effects of exposure to pesticides especially for children.

This study was conducted to evaluate the adsorbent characteristics of two mycotoxin binders (BBAc - composed of bentonite, β-glucans, and activated charcoal, and SepHt - composed of heat-treated sepiolite) against deoxynivalenol (DON) and fumonisin B₁ (FB₁) using Brunaeur-Emmett-Teller, Dubinin-Radushkevich, Freundlich, and Langmuir isotherm models and linear regression equations. Both products were tested in vitro at 0.5% with increasing levels of DON or FB₁ (0.5-10 mg L^-1) using solutions of pH 3 and pH 6 and analysed by LC-MS/MS. FB₁ adsorption rates were not different between the products (p > 0.05) at pH 3 and pH 6. At a DON concentration of 1 mg L^-1, BBAc had higher (p < 0.05) adsorption rates than SepHt. For DON, the Freundlich model had the best fit with BBAc at pH 3 and 6, and the Langmuir model with SepHt at both pHs. For FB₁, the Freundlich model had the best fit with BBAc and SepHt at pH 3, and the Langmuir model with both products at pH 6. All the linear regression equations had lower R² than the isotherm models. Therefore, the adsorption isotherm models provided more informative and reliable data for the mycotoxins and mycotoxin binders tested herein.