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

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.

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.

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.

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.

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.

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.

Time-of-flight mass spectrometry (TOF-MS) was used to unravel the composition of commercial polyglycerol polyricinoleate (PGPR) samples, by identifying the various molecular species present. To cover the broad range of molecular weights for the present species, a combination of three ionisation conditions was used. Species exceeding the molecular weight of pentaglycerol hexaricinoleate were difficult to detect. Over 100 molecular species were observed and identified in the analysed samples, including free polyglycerols, ricinoleates, and PGPR-esters. Commercial PGPR samples were shown to be mainly composed of esterification products of di-, tri-, and tetraglycerol, while the esterification degree mainly varied from 1 to 5. The TOF-MS analysis was proven to be reproducible with a relative standard deviation (RSD) below 2.86% for three independent measurements on different days. The method proved to be very suitable to evaluate batch-to-batch variations and to compare the composition of different types of commercial PGPR's. Moreover, this method can be applied to monitor the quality of PGPR products during the synthesis process. Furthermore, it can also provide fundamental knowledge for optimizing PGPR composition to improve its functionality.

Levels of mineral oil hydrocarbons were measured in a large range of green and roasted coffee beans or ground powder. To better understand the consumer exposure to mineral oil hydrocarbons, the transfer to the brewed coffee was assessed under three different preparations. As a result, less than 5% of mineral oil hydrocarbons were transferred to the cup. With this low transfer rate, the coffee contribution to the mineral oils daily intake can be assessed to be very low, below 0.8% of the total exposure.

Bisphenol A (BPA), a known endocrine disruptor, is commonly used in food containers and packaging. Recently, alternatives such as bisphenol AF (BPAF), bisphenol B (BPB), and bisphenol E (BPE) have been introduced to replace BPA. However, these substitutes have been reported to exhibit toxicity levels similar to BPA. In this study, we developed and validated a method for the analysis of trace bisphenols (BPA, BPAF, BPB, and BPE) in food using immunoaffinity column (IAC) clean-up. The method demonstrated satisfactory accuracy and precision. We applied this validated method to analyze 56 carbonated beverage samples and 30 canned tuna samples. In the carbonated beverages, average concentrations of BPA and BPAF were 0.4 and 0.2 μg kg^-1, respectively. In canned tuna, BPA and BPAF were found at average concentrations of 22.2 and 0.7 μg kg^-1, respectively, while BPB and BPE were not detected in any samples. Estimated exposure levels ranged from 0.13 to 0.18 ng kg bw^-1day^-1 in the general population and from 205.2 to 232.0 ng kg bw^-1day^-1 among consumers. The commercial IAC-based analytical method used in this study can contribute to the safety management of BPA, BPAF, BPB, and BPE.

This study aimed to investigate histamine exposure associated with consumption of fresh tuna and tuna-like species in West Java, and to estimate risk of Scombroid Fish Poisoning (SFP) in Indonesia. A range of species, including tuna (Thunnus spp.), bullet tuna (Auxis sp.), and skipjack (Katsuwonus pelamis) were collected from local markets and fish landing sites. Subsequently, histamine concentrations were determined using NMR analysis and exposure was calculated in mg/day for toddlers, children, and adults. The results showed that skipjack had the highest histamine exposure for all age groups, followed by bullet and regular tuna. The highest EDI for histamine was from skipjack consumption, accounting for 38.67; 37.77 and 20.74 percentage of exposure for toddlers, children and adults, respectively. These values are below the defined thresholds levels (ARfD), indicating no potential risk of acute health effect. Cooked bullet tuna and skipjack were estimated to cause similar illnesses, accounting for 6-7 cases per 100,000 individuals, which was higher than cooked tuna at 1-2 cases per 100,000 individuals. Considering the preparation of raw tuna in restaurants following Good Hygienic Practices (GHP), the predicted annual cases decreased significantly to 4-5 cases per million individuals. This risk estimation only considered histamine levels in fresh fish, without including data from fish preparation. Therefore, further studies were recommended to estimate the risk level in raw/fresh tuna and similar species before consumption.