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

Guazatine, a non-invasive disinfectant used for seed treatment and post-harvest citrus protection, inhibits bacterial lipid synthesis and consists of about 13 components. While it may occasionally be detected in fruits and vegetables such as citrus, its use as a pesticide has been banned in several countries due to health and environmental concerns. To ensure safe export of domestic produce, a simultaneous method of analysis for guazatine components was developed, focusing on GG, GGG, GGN, and GNG as indicators. Using LC-MS/MS, samples were extracted with a 3% formic acid/acetone mixture and purified with hexane. The method was validated across five agricultural products (mandarin, pepper, potato, brown rice, and soybean), achieving an r² above 0.995, and detection and quantitation limits of 0.8 and 2.5 µg/L, respectively. Ion suppression was high, with matrix effects ranging from -84.2 to -89.8%. Recovery rates were 70.2-99.6%, with relative standard deviations under 6.8%. Cross-laboratory validation showed recovery rates of 70.3-106.7% and relative standard deviations below 15.0%, meeting CODEX guidelines.

In recent years, food fraud issues related to whey protein supplements have disrupted the market and caused significant concern among consumers. Conventional analytical methods such as HPLC and ion exchange chromatography are commonly used to detect adulteration in whey protein supplements. However, these methods are costly, time-consuming and require specialised operation, making them less suitable for a wider range of users. This study presents a rapid and reliable approach for verifying the authenticity of whey protein supplements using laser-induced breakdown spectroscopy (LIBS) and machine learning. Specifically, this approach is employed to identify 15 brands of whey protein concentration (WPC), quantify protein and carbohydrate concentrations, distinguish three types of adulterants, and predict the level of adulteration. The relationship between LIBS data and analyte labels is established using machine learning methods, including partial least squares regression (PLSR), partial least squares discriminant analysis (PLS-DA), and kernel extreme learning machine (K-ELM). The accuracy for identifying WPC brands was over 0.977, and the highest coefficient of determination (R²) for quantifying protein and carbohydrate contents was 0.984 and 0.978, respectively. In addition, different adulterants can be differentiated with accuracies exceeding 0.986, and the R² values for adulteration prediction are above 0.967 in most cases. These results suggest that LIBS combined with machine learning can serve as a viable and efficient solution for detecting adulteration in whey protein supplements.

The present study evaluated the preparation of L-cysteine capped Fe₃O₄ (magnetite) nanoparticles (LCys-Fe₃O₄ NPs), with a particular focus on their potential as an adsorbent and also the efficiency of these NPs in the removal of patulin from apple juice. The methods employed, including Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray powder diffraction analysis (XRD), X-ray Photoelectron Spectroscopy (XPS), and Fourier Transform Infrared Spectroscopy (FT-IR), effectively showed the synthesis of LCys-Fe₃O₄ NPs. The proposed method was not only used for patulin removal; rather, it significantly enhanced the sensitivity of patulin measurement. The efficiency of patulin elimination was affected by many factors, including contact time (5-140 min), patulin initial concentration (50-150 µg/L), and amount of NPs (1-5 mg). The synthesized adsorbent achieved a removal efficiency of 98.6% for patulin adsorption at pH = 3.8. This was accomplished by employing 3 mg LCys-Fe₃O₄ NPs over a 100-min duration, resulting in a maximum adsorption capacity of 454 µg/g for the initial concentration of patulin 50 µg/L. This high removal efficiency can be attributed to active surface sites (-NH₂ and -COOH groups). The removal information obtained from an HPLC method, using the prepared adsorbent, exhibited a good fit with the Freundlich isotherm, indicating a multi-layer adsorption process on the adsorbent. The experimental findings were analyzed using an adsorption kinetic model, revealing that the adsorption kinetics of patulin onto LCys-Fe₃O₄ NPs conformed to the pseudo-second-order model. In conclusion, the proposed method demonstrated remarkable efficacy in decreasing patulin concentrations in contaminated apple juice by approximately 81.5%. Moreover, the adsorption process had no impact on the quality of the apple juice.

Aflatoxin M₁ (AFM1) is a potent mycotoxin that can contaminate milk and dairy products. It is a metabolite of aflatoxin B₁ (AFB1), which is produced by certain fungi that infect crops. In Lebanon, traditional dairy production-including various cheeses, yogurt, and Labneh-is widely practiced. However, there is limited information on how AFM1 transfers and behaves in these products. This study aimed to fill that knowledge gap by examining the transfer of AFM1 from artificially contaminated milk into traditional Lebanese dairy products, specifically Halloumi, Akkawi, double-cream, Baladiyeh cheese, yogurt, and Labneh. Milk was contaminated with a known concentration of AFM1, and the resulting dairy products were analysed for AFM1 transfer rates, focusing on the distribution between whey and curd. The study also assessed the effect of brine storage (10%) on AFM1 levels in cheese. The findings showed that the transfer of AFM1 varied depending on the processing method and type of product. Generally, whey had higher concentrations of AFM1 compared to curd. Brine storage reduced AFM1 levels in most cheese types, with the exception of double-cream cheese. Yogurt processing was found to decrease AFM1 content, while converting yogurt to Labneh resulted in an increase. This research provides valuable insights into the risk of AFM1 contamination in traditional Lebanese dairy products. Understanding the transfer and behaviour of AFM1 is essential for developing effective strategies to mitigate the risks associated with mycotoxin exposure. Accordingly, this paper also includes a risk assessment generated using the reported transfer rates that showed that dairy products produced from raw milk contaminated at 0.05 µg/L would present a high risk to the Lebanese consumer that emphasises the importance of keeping AFM1 in food at a level that is 'As Low As Reasonably Achievable' specifically in a country such as Lebanon where dairy products are highly consumed.

In the process of a routine illegal adulterant inspection of food products sold online, a suspicious compound was detected in a dried plum food product, which claimed to have a natural weight loss effect. After mass spectrometric analysis the similarity between MS/MS peaks of this compound and that of bisacodyl, it was hypothesized to be a bisacodyl derivative. The chemical structure of the unknown compound was characterized by ultra-HPLC with quadrupole time-of-flight tandem mass spectrometry (UHPLC/Q-TOF MS), HPLC-diode array detection (HPLC-DAD) and nuclear magnetic resonance (NMR) methods. Based on these results, it was confirmed that the unknown compound had the substitution of two acetyl groups in bisacodyl by two cyclopropanecarbonyl groups, respectively. This distinctive compound has been termed as bisacodyl dicycloproyl carboxylate. The new compound has not been reported yet, and therefore the detection of bisacodyl analogue should be included in routine inspection of diet foods and health products.

The presence of chloropropanols in edible oils is a significant food safety concern. Chloride in crude palm oil (CPO) is a precursor to the formation of 3-monochloropropane-1,2-diol esters (3-MCPDE) during refining; chloride retention during storage prior to refining remains under investigation. The study examined the impact of different washing treatments and storage duration on total chloride content (TCC), moisture and impurities (M&I), free fatty acid content (FFA), diacylglycerol (DAG), deterioration of bleachability index (DOBI), and iodine value (IV) of CPO. It was demonstrated that washing CPO with distilled water and 3% citric acid (DW+CA) resulted in the highest chloride reduction (37%) after one month of storage. A linear relationship was observed between TCC and FFA levels in the washed CPO, indicating that FFA is a strong predictor of chloride content. The DW+CA treatment also demonstrated a stabilizing effect on FFA levels, potentially mitigating oil deterioration during storage. These findings suggest that implementing DW+CA washing before CPO storage can effectively reduce chloride levels, enhancing the safety and quality of the oil and mitigating the risk of 3MCPDE formation during refining.

The intake of seven sweeteners (acesulfame K, aspartame, cyclamates, saccharins, steviol glycosides, sucralose (all chronic intake) and erythritol (acute intake)) via foods and beverages by the Dutch population was assessed in a refined assessment using branded data (product labels, use levels and consumption shares of brands) and scenarios for brand-loyalty. In general, the intake of these sweeteners was below their respective health-based guidance values (HBGVs). Only for toddlers high intakes of acesulfame K, cyclamates and erythritol were around or slightly above the HBGV in the most conservative scenario ('full brand-loyalty, consumers only'). However, intake of all sweeteners was likely overestimated due to conservative assumptions when data on the presence of sweeteners were absent. Improved information, particularly on products with a high contribution to the sweetener intake in toddlers, is needed to further refine the intake assessment. In conclusion, the intake of all sweeteners via foods and beverages is most likely of no concern for the Dutch population.

Citrus fruits, known for their vibrant flavours and health benefits, are susceptible to fungal attacks, particularly from toxigenic Penicillium fungi, which pose a significant pre- and post-harvest hazard. However, aromatic oils and their nanoparticles may effectively address this issue. Marjoram and fennel oils, alongside their nanoparticles, were extracted, and their aromatic constituents and antimicrobial activities were evaluated. A simulated medium with fungal spores was used to assess anti-toxigenic activity, and a simulated infection experiment was conducted with orange and lemon fruits. The capacity and mechanisms of aromatic constituents were analysed through molecular docking assays targeting enzymes involved in fungal growth and mycotoxin production. The nanoparticles exhibited good stability (89.17%-92.41%) and compact formulation (density of 0.92-0.96 g/mL). Results demonstrated substantial effectiveness of nano-emulsions against toxigenic fungi, with major aromatic compounds identified as terpinene-4-ol (18%) and γ-terpinene (11%) in marjoram and estragole (38%) and anethole (29%) in fennel oil. Diffusion assays revealed significant anti-pathogen effects (8.33-11 mm) and antifungal activity (33.33 ± 2.88-89.33 ± 1.15 mm) of marjoram and fennel nano-emulsions. Results regarding simulated infected fruit reflect spoilage delay without impacting fruit quality or sensory. The interactions between oil or nano-emulsions and fungal enzymes showed strong binding-free energy values, with significant docking scores (-6.6 to -7.0 kcal/mol) for aromatic constituents. In conclusion, aromatic antifungals offer a promising strategy for controlling Penicillium, enhancing the safety and quality of oranges and lemons, with oil nanoparticles improving antifungal efficacy by significantly reducing mycelium weight and spore germination.

Cattle grazing in the Dutch floodplains are exposed to polychlorinated dibenzo-p-dioxins and dibenzofurans (dioxins) and dioxin-like PCBs (dl-PCBs) through the consumption of grass and adhering soil. This can lead to elevated dioxin and dl-PCB levels in meat fat. To manage this contamination issue, the kinetics of these compounds in cattle need to be better understood. This study describes the development and application of a physiologically based kinetic (PBK) model to predict dioxin and dl-PCB levels in muscle fat of 'Rode Geus' cattle based on measured levels in grass and soil. Calibration of the model was performed separately for each congener, using measured dioxin and dl-PCB levels in various tissues of 14 animals. Model validation performed using dioxin and dl-PCB samples of 14 other cattle, showed that PBK model predictions were on average a factor 2.4 higher than the measured dioxin and dl-PCB TEQ levels in fat. Despite this difference, the model may still be particularly useful to better understand the relation between environmental dioxin and dl-PCB levels and those in cattle. The model is publicly available with a user-friendly interface on www.feedfoodtransfer.nl and may provide relevant insights for risk assessment and risk management.

Phthalate esters (PAEs), commonly used in food packaging materials, pose a potential health risk due to their migration into food matrices. Propolis, a resinous bee product widely consumed for its health benefits, is often packaged in plastics, raising concerns about PAE contamination. However, the occurrence of PAEs within propolis has been scarcely investigated. This study quantified PAE contamination profiles in propolis ethanolic extracts (PE) and propolis capsules (PCs) from China. The GC-MS/MS analysis of 20 PAEs demonstrated high linearity, indicating the reliability of the method. The limits of quantification (LOQ) ranged from 1.3 to 26.2 µg/kg, and the limits of detection (LOD) ranged from 0.4 to 8.6 µg/kg. Matrix effects ranged between 9% and 33%. Five PAEs were detected in PE samples: dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DiBP), dibutyl phthalate (DBP) and bis(2-ethylhexyl)phthalate (DEHP). Seventeen PAEs were detected in PC samples, with 15 consistently present in all samples (100% positivity). Diallyl phthalate (DAP), dipropyl phthalate (DPrP) and di-n-octyl phthalate (DNOP) were not detected in any sample. The total mean concentration of the 17 detected PAEs (∑17 PAEs) in the capsules ranged from 0.87 mg/kg to 23.71 mg/kg. This study found that PE and PC had the highest DBP (0.24 mg/kg) and di-heptyl phthalate (DHP: 2.29 mg/kg) levels on average, respectively. While PC showed higher PAE levels than PE. Therefore, this study provides insight into PAE contamination of raw propolis extract and encapsulated propolis.