Emerging Trends in Biogenic Amines Analysis

Biogenic amines are low-molecular-mass substances, essential for proper health for all organisms. These compounds could be detrimental to human health with various toxicological effects when they are present in high concentrations. Therefore, biogenic amines monitoring in food samples is a matter of utmost importance, and their accurate determination is considered indispensable. Under this context, we provide an overview over the most widely employed analytical techniques for biogenic amines determination such as chromatographic techniques and biosensors, emphasizing on new approaches. A critical comparison of the techniques is also given, presenting their advantages and drawbacks regarding important analytical characteristics such as sensitivity. Finally, we focus on foods in which biogenic amines mainly occur such as fish, meat and wine and other fermented products

Comprehensive overview of the analytical methods for determining pyrrolizidine alkaloids and their derived oxides in foods

Producción CientíficaPyrrolizidine alkaloids and their derived oxides are toxins naturally produced by plants when they are exposed to stress factors. In particular, the unsaturated pyrrolizidine alkaloids exhibiting a double bond between the 1,2-positions have caused great interest in recent years since they have pneumotoxic, genotoxic and carcinogenic effects upon ingestion. In this review, focus on their chemical structure justifying their toxicity is provided as well as insight on the recently adopted EU regulatory framework. In addition, to reveal current trends and highlight the research effort in the field, an all-time bibliometric analysis was performed for the first time. It was found that tea, infusions, honey, spices, and cereals are the most common foodstuffs in which pyrrolizidine alkaloids have been detected. In terms of pre-analytical steps, the application of efficient sample preparation is necessary to detect pyrrolizidine alkaloids in complex food matrices. Solvent extraction followed by a clean-up stage, e.g., solid-phase extraction was the most applied option. Focusing on the analytical methods, liquid chromatography combined with various mass spectrometry detectors has been the golden standard in the field. Gas chromatography methods were also applied, but the need for analyte derivatisation has hindered their application. All in all, this review provides an overview on the analysis of pyrrolizidine alkaloids and their derived oxides, comprehensively discussing the up-to-date advances and highlighting the analytical challenges to be faced.METROFOOD-CZ research infrastructure project (MEYS Grant No: LM2018100

Thorough investigation of the phenolic profile of reputable Greek honey varieties:varietal discrimination and floral markers identification using liquid chromatography–high-resolution mass spectrometry

Honey is a highly consumed commodity due to its potential health benefits upon certain consumption, resulting in a high market price. This fact indicates the need to protect honey from fraudulent acts by delivering comprehensive analytical methodologies. In this study, targeted, suspect and non-targeted metabolomic workflows were applied to identify botanical origin markers of Greek honey. Blossom honey samples (n = 62) and the unifloral fir (n = 10), oak (n = 24), pine (n = 39) and thyme (n = 34) honeys were analyzed using an ultra-high-performance liquid chromatography hybrid quadrupole time-of-flight mass spectrometry (UHPLC-q-TOF-MS) system. Several potential authenticity markers were revealed from the application of different metabolomic workflows. In detail, based on quantitative targeted analysis, three blossom honey markers were found, namely, galangin, pinocembrin and chrysin, while gallic acid concentration was found to be significantly higher in oak honey. Using suspect screening workflow, 12 additional bioactive compounds were identified and semi-quantified, achieving comprehensive metabolomic honey characterization. Lastly, by combining non-targeted screening with advanced chemometrics, it was possible to discriminate thyme from blossom honey and develop binary discriminatory models with high predictive power. In conclusion, a holistic approach to assessing the botanical origin of Greek honey is presented, highlighting the complementarity of the three applied metabolomic approaches

A Hybrid Lab-on-a-Chip Injector System for Autonomous Carbofuran Screening

Securing food safety standards is crucial to protect the population from health-threatening food contaminants. In the case of pesticide residues, reference procedures typically find less than 1% of tested samples being contaminated, thus indicating the necessity for new tools able to support smart and affordable prescreening. Here, we introduce a hybrid paper–lab-on-a-chip platform, which integrates on-demand injectors to perform multiple step protocols in a single disposable device. Simultaneous detection of enzymatic color response in sample and reference cells, using a regular smartphone, enabled semiquantitative detection of carbofuran, a neurotoxic and EU-banned carbamate pesticide, in a wide concentration range. The resulting evaluation procedure is generic and allows the rejection of spurious measurements based on their dynamic responses, and was effectively applied for the binary detection of carbofuran in apple extracts

Optical Screening Methods for Pesticide Residue Detection in Food Matrices: Advances and Emerging Analytical Trends

Pesticides have been extensively used in agriculture to protect crops and enhance their yields, indicating the need to monitor for their toxic residues in foodstuff. To achieve that, chromatographic methods coupled to mass spectrometry is the common analytical approach, combining low limits of detection, wide linear ranges, and high accuracy. However, these methods are also quite expensive, time-consuming, and require highly skilled personnel, indicating the need to seek for alternatives providing simple, low-cost, rapid, and on-site results. In this study, we critically review the available screening methods for pesticide residues on the basis of optical detection during the period 2016–2020. Optical biosensors are commonly miniaturized analytical platforms introducing the point-of-care (POC) era in the field. Various optical detection principles have been utilized, namely, colorimetry, fluorescence (FL), surface plasmon resonance (SPR), and surface enhanced Raman spectroscopy (SERS). Nanomaterials can significantly enhance optical detection performance and handheld platforms, for example, handheld SERS devices can revolutionize testing. The hyphenation of optical assays to smartphones is also underlined as it enables unprecedented features such as one-click results using smartphone apps or online result communication. All in all, despite being in an early stage facing several challenges, i.e., long sample preparation protocols or interphone variation results, such POC diagnostics pave a new road into the food safety field in which analysis cost will be reduced and a more intensive testing will be achieved

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

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

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

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

Honey Phenolic Compound Profiling and Authenticity Assessment Using HRMS Targeted and Untargeted Metabolomics

Honey consumption is attributed to potentially advantageous effects on human health due to its antioxidant capacity as well as anti-inflammatory and antimicrobial activity, which are mainly related to phenolic compound content. Phenolic compounds are secondary metabolites of plants, and their content in honey is primarily affected by the botanical and geographical origin. In this study, a high-resolution mass spectrometry (HRMS) method was applied to determine the phenolic profile of various honey matrices and investigate authenticity markers. A fruitful sample set was collected, including honey from 10 different botanical sources (n = 51) originating from Greece and Poland. Generic liquid–liquid extraction using ethyl acetate as the extractant was used to apply targeted and non-targeted workflows simultaneously. The method was fully validated according to the Eurachem guidelines, and it demonstrated high accuracy, precision, and sensitivity resulting in the detection of 11 target analytes in the samples. Suspect screening identified 16 bioactive compounds in at least one sample, with abscisic acid isomers being the most abundant in arbutus honey. Importantly, 10 markers related to honey geographical origin were revealed through non-targeted screening and the application of advanced chemometric tools. In conclusion, authenticity markers and discrimination patterns were emerged using targeted and non-targeted workflows, indicating the impact of this study on food authenticity and metabolomic fields