Advanced Detection and Analysis Technology for Food Contaminants and Toxicants

A special issue of Foods (ISSN 2304-8158). This special issue belongs to the section "Food Analytical Methods".

Deadline for manuscript submissions: closed (30 June 2024) | Viewed by 11337

Special Issue Editors


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Guest Editor
Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, 28933 Móstoles, Spain
Interests: contaminants; bioactive compounds; natural toxins; miniaturization; microextraction; sample preparation; liquid chromatography; mass spectrometry; novel sorbents; analytical methods
Special Issues, Collections and Topics in MDPI journals

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Guest Editor
ESCET—Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, 28933 Móstoles, Spain
Interests: contaminants; bioactive compounds; natural toxins; sample preparation; novel materials as sorbents; miniaturization; microextraction; liquid chromatography; mass spectrometry; validated analytical methods; electrochemical sensors; food control; food quality
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Currently, there are still many issues to be resolved in food safety. Accordingly, among the 17 Sustainable Development Goals (SDGs) included in the 2030 Agenda for Sustainable Development, the targets of SDG No. 2 (zero hunger) include achieving food safety and improving nutrition, mainly for the poor and people in vulnerable situations, as exposure of the population to contaminants through food can cause immediate disease and economic damage. The presence of contaminants in food is an issue to which authorities have paid close attention in recent years, so much so that regulations establishing maximum concentration limits for these compounds in some foods are being continuously published. This Special Issue will focus on analyzing food contaminants, including natural toxins, in food matrices by applying advanced analytical methodologies based on chromatographic techniques combined with mass spectrometry.

Original and review papers exploring all aspects of “Advanced Detection and Analysis Technology for Food Contaminants and Toxicants” are welcome for inclusion in this Special Issue of Foods. The papers should focus on the development of methods for the detection and quantitation of contaminants (process contaminants, environmental pollutants, veterinary drug residues, etc.) and toxins (mycotoxins, alkaloids, marine biotoxins, etc.) in foods, including new sample preparation techniques based on the use of new sorbent materials and miniaturized protocols.

We look forward to receiving your contributions.

Prof. Dr. Isabel Sierra Alonso
Prof. Dr. Sonia Morante Zarcero
Guest Editors

Manuscript Submission Information

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Keywords

  • food safety
  • food contaminants
  • toxins
  • sample preparation
  • liquid chromatography
  • gas chromatography
  • mass spectrometry
  • novel sorbents
  • analytical methods

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Published Papers (8 papers)

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Research

14 pages, 2851 KiB  
Article
Total Deoxynivalenol Contamination of Wheat Products and Coarse Grains in Shanghai, China: Occurrence and Health Risk Assessment
by Anqi Xu, Shenghao Yu, Yiqi Li, Hong Liu, Zheng Yan, Aibo Wu, Shaojie Peng and Na Liu
Foods 2024, 13(21), 3373; https://doi.org/10.3390/foods13213373 - 23 Oct 2024
Viewed by 718
Abstract
Deoxynivalenol (DON) is an important mycotoxin produced by Fusarium spp., typically found in cereals, which has garnered considerable research attention. However, the risk assessment of DON exposure to muti-cereal is partial and biased, especially lacking the evaluation of different coarse grains. In this [...] Read more.
Deoxynivalenol (DON) is an important mycotoxin produced by Fusarium spp., typically found in cereals, which has garnered considerable research attention. However, the risk assessment of DON exposure to muti-cereal is partial and biased, especially lacking the evaluation of different coarse grains. In this study, we synthesized and compared the presence of the total deoxynivalenol (free, acetylated, and masked) of a total of 372 grain samples (17 different types) based on high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS), as well as assessed the chronic and acute risks of total DON exposure in the Chinese population. DON was found at the highest frequency with an occurrence of 85.8% (319/372), followed by D3G at 17.2% (64/372). In total, 88.7% (330/372) of the grains were co-contaminated with mycotoxins. The DON and D3G contamination correlation coefficient was 0.68 in wheat flour. Moreover, different DON contamination levels were found in black beans (133.5 µg/kg), soybeans (128.7 µg/kg), and black rice (122.1 µg/kg). The DON/D3G/15A/tDON contamination level was significant differently among different coarse grains. Notably, the Monte Carlo model showed that 3.2–5.9% of adolescents consuming wheat flour and noodles suffered a chronic tDON risk. Full article
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17 pages, 4169 KiB  
Article
Simultaneous Determination of 23 Pyrrolizidine and Tropane Alkaloids in Infusions from Dry Edible Flowers Using Optimized μSPEed® Microextraction Prior to Their Analysis by UHPLC-IT-MS/MS
by Begoña Fernández-Pintor, Sonia Morante-Zarcero and Isabel Sierra
Foods 2024, 13(11), 1740; https://doi.org/10.3390/foods13111740 - 1 Jun 2024
Viewed by 1037
Abstract
A miniaturized solid-phase extraction of two tropane alkaloids (TAs) and twenty-one pyrrolizidine alkaloids (PAs) from infusions of dry edible flowers using optimized µSPEed® technique was developed. The optimization of the µSPEed® methodology involved testing different cartridges and comparing various volumes and [...] Read more.
A miniaturized solid-phase extraction of two tropane alkaloids (TAs) and twenty-one pyrrolizidine alkaloids (PAs) from infusions of dry edible flowers using optimized µSPEed® technique was developed. The optimization of the µSPEed® methodology involved testing different cartridges and comparing various volumes and numbers of loading cycles. The final conditions allowed for a rapid extraction, taking only 3.5 min. This was achieved using a C18-ODS cartridge, conditioning with 100 µL of methanol (two cycles), loading 100 µL of the infusion sample (seven cycles), and eluting the analytes with 100 µL of methanol (two cycles). Prior to their analysis by UHPLC-IT-MS/MS, the extracts were evaporated and reconstituted in 100 µL of water (0.2% formic acid)/methanol (0.2% ammonia) 95:5 (v/v), allowing for a preconcentration factor of seven times. The methodology was successfully validated obtaining recoveries ranging between 87 and 97%, RSD of less than 12%, and MQL between 0.09 and 0.2 µg/L. The validated methodology was applied to twenty samples of edible flower infusions to evaluate the safety of these products. Two infusion samples obtained from Acmella oleracea and Viola tricolor were contaminated with 0.16 and 0.2 µg/L of scopolamine (TA), respectively, while the infusion of Citrus aurantium was contaminated with intermedine and lycopsamine (PAs) below the MQL. Full article
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13 pages, 551 KiB  
Article
Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
by Osama I. Abdallah, Rania M. Abd El-Hamid, Nevein S. Ahmed, Saleh S. Alhewairini and Sherif B. Abdel Ghani
Foods 2024, 13(7), 1106; https://doi.org/10.3390/foods13071106 - 4 Apr 2024
Cited by 3 | Viewed by 1074
Abstract
A facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accuracy [...] Read more.
A facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accuracy values were between 99.8% (thiamethoxam) and 106.8% (clothianidin) at the spiking levels of 0.01, 0.1, and 1 mg/kg in the tested matrices. The precision as pooled RSD values was ≤6.1% (intra-day) and ≤6.9% (inter-day). The limit of quantification was set and tested at 0.01 mg/kg. The matrix effect was evaluated, and all matrices had a suppressive effect. The matrix of the cucumber was the most effective, with −20.9% for dinotefuran and an average of −9.8% for all compounds, while the tomato matrix had the slightest effect. Real marketed samples were analyzed using the developed and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methods; the results were not significantly different. A supervised field trial was conducted in the open field to study the dissipation patterns of imidacloprid and dinotefuran in tomatoes. The dissipation of both compounds followed first-order kinetics. The half-life (T½) values were 3.4 and 2.5 days, with dissipation rates k of 0.2013 and 0.2781 days, respectively. Following the EU-MRL database, the calculated pre-harvest interval (PHI) values were 7 and 14 days for imidacloprid and dinotefuran, respectively, and 3 days for both compounds following Codex Alimentarius regulations. The risk of imidacloprid and dinotefuran residues was estimated from chronic and acute perspectives. The risk factors of dinotefuran were lower than those of imidacloprid. Nonetheless, the highest expected residues of both compounds were below the tolerance limits. Full article
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13 pages, 2345 KiB  
Article
Ultrasensitive Ochratoxin A Detection in Cereal Products Using a Fluorescent Aptasensor Based on RecJf Exonuclease-Assisted Target Recycling
by Yanxuan Li, Furong Shao, Jin Wu, Mingzhu Liu, Gaofang Cao, Zunquan Zhao, Jialei Bai and Zhixian Gao
Foods 2024, 13(4), 595; https://doi.org/10.3390/foods13040595 - 16 Feb 2024
Viewed by 1107
Abstract
Ochratoxin A (OTA) is a mycotoxin widely found in foodstuffs such as cereal grains. It greatly threatens human health owing to its strong toxicity and high stability. Aptasensors have emerged as promising tools for the analysis of small molecule contaminants. Nucleic-acid-based signal amplification [...] Read more.
Ochratoxin A (OTA) is a mycotoxin widely found in foodstuffs such as cereal grains. It greatly threatens human health owing to its strong toxicity and high stability. Aptasensors have emerged as promising tools for the analysis of small molecule contaminants. Nucleic-acid-based signal amplification enables detectable signals to be obtained from aptasensors. However, this strategy often requires the use of complex primers or multiple enzymes, entailing problems such as complex system instability. Herein, we propose a fluorescent aptasensor for the ultrasensitive detection of OTA in cereal products, with signal amplification through RecJf exonuclease-assisted target recycling. The aptamer/fluorescein-labeled complementary DNA (cDNA-FAM) duplex was effectively used as the target-recognition unit as well as the potential substrate for RecJf exonuclease cleavage. When the target invaded the aptamer-cDNA-FAM duplex to release cDNA-FAM, RecJf exonuclease could cleave the aptamer bonded with the target and release the target. Thus, the target-triggered cleavage cycling would continuously generate cDNA-FAM as a signaling group, specifically amplifying the response signal. The proposed exonuclease-assisted fluorescent aptasensor exhibited a good linear relationship with OTA concentration in the range from 1 pg/mL to 10 ng/mL with an ultralow limit of detection (6.2 ng/kg of cereal). The analytical method showed that recoveries of the cereal samples ranged from 83.7 to 109.3% with a repeatability relative standard deviation below 8%. Importantly, the proposed strategy is expected to become a common detection model because it can be adapted for other targets by replacing the aptamer. Thus, this model can guide the development of facile approaches for point-of-care testing applications. Full article
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11 pages, 8357 KiB  
Article
Assessing Matrix Solid-Phase Dispersion Extraction Strategies for Determining Bisphenols and Phthalates in Gilthead Sea Bream Samples
by Dulce L. Soliz, Rosa Ma Garcinuño, Gema Paniagua González, Juan Carlos Bravo and Pilar Fernández Hernando
Foods 2024, 13(3), 413; https://doi.org/10.3390/foods13030413 - 27 Jan 2024
Cited by 3 | Viewed by 1471
Abstract
Microplastics (MPs) and nanoplastics (NPs) are widely spread in the environment, generating significant concern due to their potential impact on environmental health. Marine species usually ingest plastic fragments, mistaking them for food. Many toxic compounds, such as plastic additives that are not chemically [...] Read more.
Microplastics (MPs) and nanoplastics (NPs) are widely spread in the environment, generating significant concern due to their potential impact on environmental health. Marine species usually ingest plastic fragments, mistaking them for food. Many toxic compounds, such as plastic additives that are not chemically bound to the plastic matrix, can be released from MPs and NPs and reach humans via the food chain. This paper highlights the development and validation of a straightforward solid–liquid extraction clean-up procedure in combination with a matrix solid-phase dispersion method using high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) detection, enabling facile, precise, and reliable identification and quantitation of a total of six bisphenols and phthalates in gilthead sea breams. Under the optimized conditions, the developed method showed good linearity (R2 > 0.993) for all target compounds. The recoveries obtained were between 70 and 92%. The relative standard deviations (RSDs) for reproducibility (inter-day) and repeatability (intra-day) were less than 9% and 10%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for the target compounds ranged from 0.11 to 0.68 µg/kg and from 0.37 to 2.28 µg/kg, respectively. A new, efficient extraction methodology for the determination of BPA, BPS, BPF, DBP, DEP, and DHEP in gilthead seabream has been optimized and validated. Full article
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19 pages, 4345 KiB  
Article
Determination of Eugenol Residues in Fish Tissue, Transport, and Temporary Water of Aquatic Product by Gas Chromatography–Tandem Mass Spectrometry with Application of the Electrospun Nanofibrous Membrane
by Deqian Wang, Yunning Wang, Bolin Liu, Ling Ni, Jian Zhong, Jing Xie and Zhengquan Wang
Foods 2024, 13(2), 238; https://doi.org/10.3390/foods13020238 - 11 Jan 2024
Cited by 1 | Viewed by 1433
Abstract
Using gas chromatography–tandem mass spectrometry and electrospun nanofibrous membrane, we developed and validated a simple, rapid, and sensitive methodology for quantifying eugenol residues in fish tissue and water samples. Fish tissue extract and water samples (315 samples) collected from three southeastern China provinces [...] Read more.
Using gas chromatography–tandem mass spectrometry and electrospun nanofibrous membrane, we developed and validated a simple, rapid, and sensitive methodology for quantifying eugenol residues in fish tissue and water samples. Fish tissue extract and water samples (315 samples) collected from three southeastern China provinces (Shanghai, Zhejiang, and Fujian), originating from eight provinces of Zhejiang, Jiangsu, Shandong, Guangdong, Fujian, Anhui, Shanghai, and Jiangxi, from April 2021 to April 2023 were filtered with an electrospun nanofiber membrane, extracted with trichloromethane/n-hexane, and directly concentrated to dry after simple purification. An internal standard of p-terphenyl in n-hexane and 5-µL injection volumes of the solutions was used to analyze eugenol via internal calibration with a minimum concentration of 0.5 µg/L in water samples and 0.1 µg/kg in aquatic product samples. The highest amount of eugenol was detected in Fujian province, possibly due to the higher temperature during transportation, while the lowest amount was found in Shanghai, which mainly uses temporary fish-culture devices. This is a fast, inexpensive, and effective method for testing large quantities of fish water and meat samples. Full article
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13 pages, 2516 KiB  
Article
Nondestructive and Rapid Screening of Aflatoxin-Contaminated Single Peanut Kernels Using Field-Portable Spectroscopy Instruments (FT-IR and Raman)
by Siyu Yao, Gonzalo Miyagusuku-Cruzado, Megan West, Victor Nwosu, Eric Dowd, Jake Fountain, M. Monica Giusti and Luis E. Rodriguez-Saona
Foods 2024, 13(1), 157; https://doi.org/10.3390/foods13010157 - 2 Jan 2024
Cited by 2 | Viewed by 1804
Abstract
A nondestructive and rapid classification approach was developed for identifying aflatoxin-contaminated single peanut kernels using field-portable vibrational spectroscopy instruments (FT-IR and Raman). Single peanut kernels were either spiked with an aflatoxin solution (30 ppb–400 ppb) or hexane (control), and their spectra were collected [...] Read more.
A nondestructive and rapid classification approach was developed for identifying aflatoxin-contaminated single peanut kernels using field-portable vibrational spectroscopy instruments (FT-IR and Raman). Single peanut kernels were either spiked with an aflatoxin solution (30 ppb–400 ppb) or hexane (control), and their spectra were collected via Raman and FT-IR. An uHPLC-MS/MS approach was used to verify the spiking accuracy via determining actual aflatoxin content on the surface of randomly selected peanut samples. Supervised classification using soft independent modeling of class analogies (SIMCA) showed better discrimination between aflatoxin-contaminated (30 ppb–400 ppb) and control peanuts with FT-IR compared with Raman, predicting the external validation samples with 100% accuracy. The accuracy, sensitivity, and specificity of SIMCA models generated with the portable FT-IR device outperformed the methods in other destructive studies reported in the literature, using a variety of vibrational spectroscopy benchtop systems. The discriminating power analysis showed that the bands corresponded to the C=C stretching vibrations of the ring structures of aflatoxins were most significant in explaining the variance in the model, which were also reported for Aspergillus-infected brown rice samples. Field-deployable vibrational spectroscopy devices can enable in situ identification of aflatoxin-contaminated peanuts to assure regulatory compliance as well as cost savings in the production of peanut products. Full article
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11 pages, 2158 KiB  
Article
Acetylcholinesterase- and Butyrylcholinesterase-Based Biosensors for the Detection of Quaternary Ammonium Biocides in Food Industry
by Lynn Mouawad, Georges Istamboulie, Gaëlle Catanante and Thierry Noguer
Foods 2024, 13(1), 133; https://doi.org/10.3390/foods13010133 - 30 Dec 2023
Cited by 2 | Viewed by 1954
Abstract
A sensitive and robust electrochemical cholinesterase-based sensor was developed to detect the quaternary ammonium (QAs) biocides most frequently found in agri-food industry wash waters: benzalkonium chloride (BAC) and didecyldimethylammonium chloride (DDAC). To reach the maximum residue limit of 28 nM imposed by the [...] Read more.
A sensitive and robust electrochemical cholinesterase-based sensor was developed to detect the quaternary ammonium (QAs) biocides most frequently found in agri-food industry wash waters: benzalkonium chloride (BAC) and didecyldimethylammonium chloride (DDAC). To reach the maximum residue limit of 28 nM imposed by the European Union (EU), two types of cholinesterases were tested, acetylcholinesterase (AChE, from Drosophila melanogaster) and butyrylcholinesterase (BChE, from horse serum). The sensors were designed by entrapping AChE or BChE on cobalt phthalocyanine-modified screen-printed carbon electrodes. The limits of detection (LOD) of the resulting biosensors were 38 nM for DDAC and 320 nM for BAC, using, respectively, AChE and BChE. A simple solid-phase extraction step was used to concentrate the samples before biosensor analysis, allowing for the accurate determination of DDAC and BAC in tap water with limits of quantification (LOQ) as low as 2.7 nM and 5.3 nM, respectively. Additional assays demonstrated that the use of a phosphotriesterase enzyme allows for the total removal of interferences due to the possible presence of organophosphate insecticides in the sample. The developed biosensors were shown to be stable during 3 months storage at 4 °C. Full article
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