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Department of Food Analysis and Nutrition, Faculty of Food and Biochemical Technology, University of Chemistry and Technology Prague, Technická 5, 166 28 Prague 6 – Dejvice, Prague, Czech Republic

Dr. Aristeidis Tsagkaris

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Department of Food Analysis and Nutrition, Faculty of Food and Biochemical Technology, University of Chemistry and Technology Prague, Technická 5, 166 28 Prague 6 – Dejvice, Prague, Czech Republic

Prof. Dr. Efstathios Z. Panagou

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Laboratory of Microbiology and Biotechnology of Foods, Department of Food Science and Human Nutrition, School of Food and Nutritional Sciences, Agricultural University of Athens, Iera Odos 75, 118 55 Athens, Greece

Instrumental and Bioanalytical Methods for Food Contaminant Detection

Abstract submission deadline

closed (30 June 2022)

Manuscript submission deadline

closed (30 September 2022)

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Topic Information

Dear Colleagues,

Food safety is of paramount importance for a wide variety of stakeholders, namely, producers, industry, governmental bodies, and citizens. However, the intensive and globalized food production indicates that food testing from farm-to-fork is a rather challenging task. In fact, although regulatory requirements are in force globally, contaminated food is still consumed, resulting in (i) health-related problems due to acute toxicity incidents, e.g., consumption of an undeclared allergen; (ii) significant financial losses as in the fipronil case (insecticide in eggs, EU, 2017); and (iii) foodborne diseases, such as salmonellosis. Therefore, the development of analytical methods capable of providing fit-for-purpose results is necessary to tackle such emerging risks. Two different types of methods (in principle complementary) have been applied, namely, instrumental analysis and screening analytical methods predominantly based on biorecognition events.

We are pleased to invite you to submit papers that showcase and discuss novel analytical methods (both instrumental and sensor-based) in the food safety field. The submitted papers should address rapid, cost-efficient, robust, and sensitive analytical procedures to allow effective testing of toxicologically relevant food contaminants. Such contaminants include chemical contaminants, such as pesticide or antibiotic residues, natural toxins, e.g., mycotoxins or marine toxins and food pathogens.

This Special Issue aims to provide a fruitful collection of papers (both original and review papers) based on (a) novel chromatographic separation methods coupled to various detectors with special emphasis to mass spectrometric (MS) detection, (b) optical and electrochemical biosensors and their potential to be hyphenated with smartphones as their analytical detector, (c) approaches to automate and miniaturize food contaminant analysis, e.g., lab-on-a-chip (LOC) assays or micro total analysis systems (μTAS), and (d) method validation and cross comparison toward golden standard methods.

We look forward to receiving your contributions.

Prof. Dr. Jana Pulkrabova
Dr. Aristeidis Tsagkaris
Prof. Dr. Efstathios Z. Panagou
Topic Editors

Keywords

chromatography
mass spectrometry
biosensors
bioassays
point-of-care/point-of-need
lab-on-a-chip
food safety
food contaminants
toxins
food pathogens
validation

Participating Journals

Journal Name	Impact Factor	CiteScore	Launched Year	First Decision (median)	APC
Microorganisms microorganisms	4.1	7.4	2013	13.4 Days	CHF 2700
Toxics toxics	3.9	4.5	2013	15.6 Days	CHF 2600
Toxins toxins	3.9	7.5	2009	18.9 Days	CHF 2700

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Published Papers (10 papers)

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12 pages, 1764 KiB

Open AccessArticle

An Improved Method for Quantification of Viable Fusarium Cells in Infected Soil Products by Propidium Monoazide Coupled with Real-Time PCR

by Lida Chen, Lei Li, Xuewen Xie, Ali Chai, Yanxia Shi, Tengfei Fan, Jianming Xie and Baoju Li

Microorganisms 2022, 10(5), 1037; https://doi.org/10.3390/microorganisms10051037 - 17 May 2022

Cited by 5 | Viewed by 2661

Abstract

Fusarium is a soil-borne pathogen that causes root rot disease in cucumber. To date, quantitative real-time PCR (qPCR) is a common tool to detect the content of Fusarium in soil. However, qPCR cannot distinguish between viable and nonviable cells. The aim of this study was to develop a detection technique to pretreat tissue fluid with propidium monoazide (PMA) followed by extract DNA, and then to quantify viable Fusarium cells in contaminated soil. In this work, the specific primer pair F8-1/F8-2 was designed based on the translation elongation factor (EF) gene and a PMA-qPCR assay was established to amplify and quantify soils of viable Fusarium cells. The PMA pretreatment test was optimized, which indicated that the optimal PMA concentration and light exposure time were 50 mmol L⁻¹ and 15 min, respectively. The lowest limit of viable cells in suspension detected and soil by PMA-qPCR were 82 spore mL⁻¹ and 91.24 spore g⁻¹, respectively. For naturally contaminated soil, viable Fusarium cells were detected in eight of the 18 samples, and the Fusarium amount ranged from 10⁴ to 10⁶ spore g⁻¹. In conclusion, the PMA-qPCR method has the characteristics of high sensitivity, efficiency, and time saving, which could support nursery plants to avoid Fusarium infection and agro-industry losses. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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11 pages, 1399 KiB

Open AccessArticle

Differentiation of Bacillus cereus and Bacillus thuringiensis Using Genome-Guided MALDI-TOF MS Based on Variations in Ribosomal Proteins

by Minling Chen, Xianhu Wei, Junhui Zhang, Huan Zhou, Nuo Chen, Juan Wang, Ying Feng, Shubo Yu, Jumei Zhang, Shi Wu, Qinghua Ye, Rui Pang, Yu Ding and Qingping Wu

Microorganisms 2022, 10(5), 918; https://doi.org/10.3390/microorganisms10050918 - 27 Apr 2022

Cited by 6 | Viewed by 3380

Abstract

Bacillus cereus and B. thuringiensis are closely related species that are relevant to foodborne diseases and biopesticides, respectively. Unambiguous differentiation of these two species is crucial for bacterial taxonomy. As genome analysis offers an objective but time-consuming classification of B. cereus and B. thuringiensis, in the present study, matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) was used to accelerate this process. By combining in silico genome analysis and MALDI-TOF MS measurements, four species-specific peaks of B. cereus and B. thuringiensis were screened and identified. The species-specific peaks of B. cereus were m/z 3211, 6427, 9188, and 9214, and the species-specific peaks of B. thuringiensis were m/z 3218, 6441, 9160, and 9229. All the above peaks represent ribosomal proteins, which are conserved and consistent with the phylogenetic relationship between B. cereus and B. thuringiensis. The specificity of the peaks was robustly verified using common foodborne pathogens. Thus, we concluded that genome-guided MALDI-TOF MS allows high-throughput differentiation of B. cereus and B. thuringiensis and provides a framework for differentiating other closely related species. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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15 pages, 616 KiB

Open AccessArticle

Preliminary Investigation of Biogenic Amines in Type I Sourdoughs Produced at Home and Bakery Level

by Giuseppe Mannino, Fortunato Cirlincione, Raimondo Gaglio, Elena Franciosi, Nicola Francesca, Giancarlo Moschetti, Alberto Asteggiano, Claudio Medana, Carla Gentile and Luca Settanni

Toxins 2022, 14(5), 293; https://doi.org/10.3390/toxins14050293 - 20 Apr 2022

Cited by 5 | Viewed by 2300

Abstract

During a survey for isolating sourdough lactic acid bacteria (LAB), 20 dough samples produced at the bakery level (BL) or home-made (HM) were collected. An enzyme-based colorimetric method revealed a total biogenic amines (BAs) concentration in the range 41.4–251.8 ppm for six (three BL and three HM) sourdoughs characterised by unpleasant odours. Eight BAs generally investigated in foods were identified and quantified from these six samples by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS). Only one HM sample contained almost all analysed BAs. Tryptamine was exclusively detected in HM sourdoughs (0.71–24.1 ppm). Putrescine, tryptamine, spermidine, and spermine were the only BAs detected in BL sourdoughs. MiSeq Illumina analysis was applied to study the total bacterial community of sourdoughs. LAB accounted from 67.89 to 92.17% of total bacterial diversity, and Levilactobacillus brevis was identified in all six sourdoughs. Leuconostoc, Pediococcus, and Weissella were also dominant. Plate counts detected neither the presence of Pseudomonas nor members of the Enterobacteriaceae family, and LAB levels were, on average, barely 5.89 Log CFU/g for BL, and 7.33 Log CFU/g for HM sourdoughs. Data suggested that the microorganisms mainly imputable of BAs formation in sourdough are members of the LAB community. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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16 pages, 1966 KiB

Open AccessArticle

Mesostructured Silicas as Cation-Exchange Sorbents in Packed or Dispersive Solid Phase Extraction for the Determination of Tropane Alkaloids in Culinary Aromatics Herbs by HPLC-MS/MS

by Lorena González-Gómez, Judith Gañán, Sonia Morante-Zarcero, Damián Pérez-Quintanilla and Isabel Sierra

Toxins 2022, 14(3), 218; https://doi.org/10.3390/toxins14030218 - 17 Mar 2022

Cited by 10 | Viewed by 5180

Abstract

In this work, Hexagonal Mesoporous Silica (HMS) and Santa Barbara Amorphous-15 (SBA-15) mesostructured silicas were synthesized and functionalized with sulfonic acid groups. The materials (HMS-SO₃⁻ and SBA-15-SO₃⁻) were evaluated as strong cation exchange sorbents for sample extract clean-up, by solid phase extraction (SPE) and dispersive solid phase extraction, to determine atropine (At) and scopolamine (Sc) in commercial culinary aromatic herbs. Under optimized conditions, 0.25 g of sample was subject to solid–liquid extraction with acidified water (pH 1.0), and good recovery percentages were achieved for At and Sc using 75 mg of HMS-SO₃⁻ in SPE as the clean-up stage, prior to their determination by HPLC-MS/MS. The proposed method was validated in a thyme sample showing recoveries in the range of 70–92%, good linearity (R² > 0.999), adequate precision (RSD ≤ 14%) and low limits (MDL 0.8–2.2 µg/kg and MQL 2.6–7.2 µg/kg for both analytes). Sixteen aromatic herbs samples (dried thyme, basil and coriander leaves) were analysed and At was found in fourteen samples over an interval of <5–42 μg/kg, whereas Sc was found in three of the sixteen samples studied (between <5–34 μg/kg). The amount of At and Sc found in some analysed samples confirms the importance of setting maximum levels of At and Sc in culinary aromatic herbs. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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22 pages, 13022 KiB

Open AccessArticle

Comparative Assessment of Antibiotic Residues Using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS) and a Rapid Screening Test in Raw Milk Collected from the North-Central Algerian Dairies

by Fawzi Rostane Meklati, Anthi Panara, Ahmed Hadef, Amel Meribai, Meriem H. Ben-Mahdi, Marilena E. Dasenaki and Nikolaos S. Thomaidis

Toxics 2022, 10(1), 19; https://doi.org/10.3390/toxics10010019 - 5 Jan 2022

Cited by 18 | Viewed by 4222

Abstract

Antibiotic residues in milk are a major health threat for the consumer and a hazard to the dairy industry, causing significant economic losses. This study aims to assess the presence of antibiotic residues in raw milk comparatively by a rapid screening test (BetaStar^® Combo) and Liquid Chromatography coupled with Tandem Mass Spectrometry (LC-MS/MS). A total of 445 samples were collected from 3 dairy companies of north-central Algeria (Algiers, Blida, Boumerdes), and they were rapidly screened for β-lactams and tetracyclines; 52 samples, comprising 34 positive tanker-truck milk and 18 negative bulk-tank milk were tested by LC-MS/MS, which revealed 90.4% were contaminated (n = 47) and 55.3% exceeded the Maximum Residue Limit (MRL). The β-lactams as parent compounds and their metabolites were the most frequently detected with maximum value for cloxacillin (1231 µg/kg) and penicillin G (2062 µg/kg). Under field condition, the false-positive results, particularly for tetracyclines, seems to be related to milk samples displaying extreme acidity values (≥19°D) or fat-level fluctuations (2.7 g/100 mL and 5.6–6.2 g/100 mL). Despite a relatively low prevalence (7.64%) of residues using the rapid test, the detection by LC-MS/MS of flumequine (52 µg/kg), cefaclor (maximum 220 µg/kg) and metabolites of β-lactams at high levels should lead to reflections on the control of their human and environmental toxicological effects. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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13 pages, 1385 KiB

Open AccessEditor’s ChoiceArticle

Critical Assessment of Clean-Up Techniques Employed in Simultaneous Analysis of Persistent Organic Pollutants and Polycyclic Aromatic Hydrocarbons in Fatty Samples

by Lucie Drábová, Darina Dvořáková, Kateřina Urbancová, Tomáš Gramblička, Jana Hajšlová and Jana Pulkrabová

Toxics 2022, 10(1), 12; https://doi.org/10.3390/toxics10010012 - 1 Jan 2022

Cited by 8 | Viewed by 2389

Abstract

Interference of residual lipids is a very common problem in ultratrace analysis of contaminants in fatty matrices. Therefore, quick and effective clean-up techniques applicable to multiple groups of analytes are much needed. Cartridge and dispersive solid-phase extraction (SPE and dSPE) are often used for this purpose. In this context, we evaluated the lipid clean-up efficiency and performance of four commonly used sorbents—silica, C18, Z-Sep, and EMR-lipid—for the determination of organic pollutants in fatty fish samples (10%) extracted using ethyl acetate or the QuEChERS method. Namely, 17 polychlorinated biphenyls (PCBs), 22 organochlorine pesticides (OCPs), 13 brominated flame retardants (BFRs), 19 per- and polyfluoroalkyl substances (PFAS), and 16 polycyclic aromatic hydrocarbons (PAHs) were determined in this study. The clean-up efficiency was evaluated by direct analysis in real time coupled with time-of-flight mass spectrometry (DART-HRMS). The triacylglycerols (TAGs) content in the purified extracts were significantly reduced. The EMR-lipid sorbent was the most efficient of the dSPE sorbents used for the determination of POPs and PAHs in this study. The recoveries of the POPs and PAHs obtained by the validated QuEChERS method followed by the dSPE EMR-lipid sorbent ranged between 59 and 120%, with repeatabilities ranging between 2 and 23% and LOQs ranging between 0.02 and 1.50 µg·kg⁻¹. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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14 pages, 823 KiB

Open AccessArticle

Regulated and Non-Regulated Mycotoxin Detection in Cereal Matrices Using an Ultra-High-Performance Liquid Chromatography High-Resolution Mass Spectrometry (UHPLC-HRMS) Method

by Aristeidis S. Tsagkaris, Nela Prusova, Zbynek Dzuman, Jana Pulkrabova and Jana Hajslova

Toxins 2021, 13(11), 783; https://doi.org/10.3390/toxins13110783 - 5 Nov 2021

Cited by 10 | Viewed by 3046

Abstract

Cereals represent a widely consumed food commodity that might be contaminated by mycotoxins, resulting not only in potential consumer health risks upon dietary exposure but also significant financial losses due to contaminated batch disposal. Thus, continuous improvement of the performance characteristics of methods to enable an effective monitoring of such contaminants in food supply is highly needed. In this study, an ultra-high-performance liquid chromatography coupled to a hybrid quadrupole orbitrap mass analyzer (UHPLC-q-Orbitrap MS) method was optimized and validated in wheat, maize and rye flour matrices. Nineteen analytes were monitored, including both regulated mycotoxins, e.g., ochratoxin A (OTA) or deoxynivalenol (DON), and non-regulated mycotoxins, such as ergot alkaloids (EAs), which are analytes that are expected to be regulated soon in the EU. Low limits of quantification (LOQ) at the part per trillion level were achieved as well as wide linear ranges (four orders of magnitude) and recovery rates within the 68–104% range. Overall, the developed method attained fit-for-purpose results and it highlights the applicability of high-resolution mass spectrometry (HRMS) detection in mycotoxin food analysis. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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10 pages, 3443 KiB

Open AccessArticle

Dramatically Enhancing the Sensitivity of Immunoassay for Ochratoxin A Detection by Cascade-Amplifying Enzyme Loading

by Zhuolin Song, Lin Feng, Yuankui Leng, Mingzhu Huang, Hao Fang, Weipeng Tong, Xuelan Chen and Yonghua Xiong

Toxins 2021, 13(11), 781; https://doi.org/10.3390/toxins13110781 - 5 Nov 2021

Cited by 8 | Viewed by 2575

Abstract

Enzyme-linked immunosorbent assay (ELISA) is widely used in the routine screening of mycotoxin contamination in various agricultural and food products. Herein, a cascade-amplifying system was introduced to dramatically promote the sensitivity of an immunoassay for ochratoxin A (OTA) detection. Specifically, a biotinylated M13 bacteriophage was introduced as a biofunctional competing antigen, in which a seven-peptide OTA mimotope fused on the p3 protein of M13 was used to specifically recognize an anti-OTA monoclonal antibody, and the biotin molecules modified on capsid p8 proteins were used in loading numerous streptavidin-labeled polymeric horseradish peroxidases (HRPs). Owing to the abundance of biotinylated p8 proteins in M13 and the high molar ratio between HRP and streptavidin in streptavidin-polyHRP, the loading amount of HRP enzymes on the M13 bacteriophage were greatly boosted. Hence, the proposed method exhibited high sensitivity, with a limit of detection of 2.0 pg/mL for OTA detection, which was 250-fold lower than that of conventional ELISA. In addition, the proposed method showed a slight cross-reaction of 2.3% to OTB, a negligible cross-reaction for other common mycotoxins, and an acceptable accuracy for OTA quantitative detection in real corn samples. The practicability of the method was further confirmed with a traditional HRP-based ELISA method. In conclusion, the biotinylated bacteriophage and polyHRP structure showed potential as a cascade-amplifying enzyme loading system for ultra-trace OTA detemination, and its application can be extended to the detection of other analytes by altering specific mimic peptide sequences. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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34 pages, 4732 KiB

Open AccessArticle

Extraction and LC-MS/MS Analysis of Ciguatoxins: A Semi-Targeted Approach Designed for Fish of Unknown Origin

by Astrid Spielmeyer, Christopher R. Loeffler and Dorina Bodi

Toxins 2021, 13(9), 630; https://doi.org/10.3390/toxins13090630 - 8 Sep 2021

Cited by 11 | Viewed by 3824

Abstract

Ciguatoxins (CTXs) are polyether marine biotoxins that can cause ciguatera poisoning (CP) after the consumption of fish or invertebrates containing sub ppb levels; concentrations that present a challenge for current extraction and analysis methods. Here, a newly developed and (partly) validated single-day extraction protocol is presented. First, the fish sample is broken-down by enzymatic digestion, followed by extraction and extract clean-up by defatting and two solid-phase extractions. Final extracts were investigated using two different CTX-analysis methods; an in vitro cytotoxicity assay (N2a-assay) and by LC-MS/MS. Validation was performed for both fillet and freeze-dried samples of snapper, parrotfish, and grouper spiked with CTX1B, 52-epi-54-deoxyCTX1B, 54-deoxyCTX1B, and CTX3C. Based on recovery rates (35–88%) and matrix effects (66–116%) determined by LC-MS/MS, the enzyme protocol is applicable to various matrices. The protocol was applied to naturally contaminated fish tissue (Lutjanus bohar) obtained during a CP incident in Germany. Several potential CTX congeners were identified by a two-tier LC-MS/MS approach (screening of sodium adducts, high-resolution or low-resolution confirmation via ammonium adducts). Inclusion of >30 known CTX congeners into the LC-MS/MS methods and single-day sample preparation make the method suitable for analysis of ciguatera suspect samples at sub ppb levels also with undisclosed CTX profiles. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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20 pages, 2328 KiB

Open AccessFeature PaperArticle

A Quantitative ¹H NMR Method for Screening Cannabinoids in CBD Oils

by Ines Barthlott, Andreas Scharinger, Patricia Golombek, Thomas Kuballa and Dirk W. Lachenmeier

Toxics 2021, 9(6), 136; https://doi.org/10.3390/toxics9060136 - 10 Jun 2021

Cited by 20 | Viewed by 5987

Abstract

Toxicologically relevant levels of the psychoactive ∆⁹-tetrahydocannabinol (∆⁹-THC) as well as high levels of non-psychoactive cannabinoids potentially occur in CBD (cannabidiol) oils. For consumer protection in the fast-growing CBD oil market, facile and rapid quantitative methods to determine the cannabinoid content are crucial. However, the current standard method, i.e., liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS), requires a time-consuming multistep sample preparation. In this study, a quantitative nuclear magnetic resonance spectroscopy (qNMR) method for screening cannabinoids in CBD oils was developed. Contrary to the HPLC-MS/MS method, this qNMR features a simple sample preparation, i.e., only diluting the CBD oil in deuterochloroform. Pulse length-based concentration determination (PULCON) enables a direct quantification using an external standard. The signal intensities of the cannabinoids were enhanced during the NMR spectra acquisition by means of multiple suppression of the triglycerides which are a major component of the CBD oil matrix. The validation confirmed linearity for CBD, cannabinol (CBN), ∆⁹-THC and ∆⁸-THC in hemp seed oil with sufficient recoveries and precision for screening. Comparing the qNMR results to HPLC-MS/MS data for 46 commercial CBD oils verified the qNMR accuracy for ∆⁹-THC and CBD, but with higher limits of detection. The developed qNMR method paves the way for increasing the sample throughput as a complementary screening before HPLC-MS/MS. Full article

(This article belongs to the Topic Instrumental and Bioanalytical Methods for Food Contaminant Detection)

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