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Pancreatic lipase (PNLIP, EC 3.1.1.3) plays a pivotal role in the digestion of dietary lipids, a metabolic pathway directly related to obesity. One of the effective strategies in obesity treatment is the inhibition of PNLIP, which is possible to be achieved by specific phenolic compounds occurring in high abundance in some plants. In this study, a multidisciplinary approach is presented investigating the PNLIP inhibitory effect of 33 plants belonging in the Asteraceae botanical family. In the first stage of the study, a rapid and cost-efficient PNLIP assay in a 96-microwell plate format was developed and important parameters were optimized, e.g., the enzyme substrate. Upon PNLIP assay optimization, aqueous and dichloromethane Asteraceae plant extracts were tested and a cut-off inhibition level was set to further analyze only the samples with a significant inhibitory effect (inhibitory rate > 40%), using an ultra-high-performance liquid chromatography hybrid quadrupole time-of-flight mass spectrometry (UHPLC-q-TOF-MS) method. Specifically, a metabolomic suspect screening was performed and 69 phenolic compounds were tentatively identified, including phenolic acids, flavonoids, flavonoid-3-O-glycosides, and flavonoid-7-O-glycosides, amongst others. In the case of aqueous extracts, phytochemicals known for inducing PNLIP inhibitory effect, e.g., compounds containing galloyl molecules or caffeoylquinic acids, were monitored in Chrysanthemum morifolium, Grindella camporum and Hieracium pilosella extracts. All in all, the presented approach combines in vitro bioactivity measurements to high-end metabolomics to identify phenolic compounds with potential medicinal and/or dietary applications.

Agricultural systems are increasingly impacted by micro- and nanoplastic (MNP) pollution raising concerns for food safety and security. To understand the scale of the problem and develop mitigation strategies, there is a need to characterise the effects and impacts of MNP. Here, we discuss the main MNP entry pathways into the human food chain and their effects/impact on food and feed sources, identifying major research gaps hindering robust risk assessments of MNP pollution. We identified emerging and current analytical methods to facilitate the closing of those gaps. An interdisciplinary approach combining omics strategies with novel methods for fast and reliable MNP measurement and plastic additive leaching characterisation across multiple dynamic environments can accurately quantify MNP pollution risks. Data of this type is essential to support policy development and legislation to prevent further MNP pollution from causing food safety and security problems worldwide.

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.

Rare Earth Elements (REEs), La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, and Y, & two actinides, Th and U were assessed in muscle and liver tissues of wild, backyard and commercially raised rabbits through ICP-MS. Higher concentrations were found in liver in comparison to muscle tissue. Liver of wild rabbits accumulates all studied elements beyond Tm. Backyard rabbits do not show any statistically significant accumulation while commercial accumulate all beyond La, Ce, Pr, Nd, Gd and Tb. Wild rabbits were with the highest amounts for most of these elements. The different living and rearing environments of wild, backyard and commercial rabbits may affect accumulation, fate and transfer of REEs in rabbits' tissues. A dataset for establishing reference values of REEs in Lemnos island wild rabbits' is shown and the literature gap on safety limits for REEs is discussed.

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.

Honey is a high-value, globally consumed, food product featuring a high market price strictly related to its origin. Moreover, honey origin has to be clearly stated on the label, and quality schemes are prescribed based on its geographical and botanical origin. Therefore, to enhance food quality, it is of utmost importance to develop analytical methods able to accurately and precisely discriminate honey origin. In this study, an all-time scientometric evaluation of the field is provided for the first time using a structured keyword on the Scopus database. The bibliometric analysis pinpoints that the botanical origin discrimination was the most studied authenticity issue, and chromatographic methods were the most frequently used for its assessment. Based on these results, we comprehensively reviewed analytical techniques that have been used in honey authenticity studies. Analytical breakthroughs and bottlenecks on methodologies to assess honey quality parameters using separation, bioanalytical, spectroscopic, elemental and isotopic techniques are presented. Emphasis is given to authenticity markers, and the necessity to apply chemometric tools to reveal them. Altogether, honey authenticity is an ever-growing field, and more advances are expected that will further secure honey quality.

The trend of the number of publications on a research field is often used to quantify research interest and effort, but this measure is biased by general publication record inflation. This study introduces a novel metric as an unbiased and quantitative tool for trend analysis and bibliometrics. The metric was used to reanalyze reported publication trends and perform in-depth trend analyses on patent groups and a broad range of field in the life-sciences. The analyses confirmed that inflation bias frequently results in the incorrect identification of field-specific increased growth. It was shown that the metric enables a more detailed, quantitative and robust trend analysis of peer reviewed publications and patents. Some examples of the metric’s uses are quantifying inflation-corrected growth in research regarding microplastics (51% ± 10%) between 2012 and 2018 and detecting inflation-corrected growth increase for transcriptomics and metabolomics compared to genomics and proteomics (Tukey post hoc p

Smartphone based devices (SBDs) have the potential to revolutionize food safety control by empowering citizens to perform screening tests. To achieve this, it is of paramount importance to understand current research efforts and identify key technology gaps. Therefore, a systematic review of optical SBDs in the food safety sector was performed. An overview of reviewed SBDs is given focusing on performance characteristics as well as image analysis procedures. The state-of-the-art on commercially available SBDs is also provided. This analysis revealed several important technology gaps, the most prominent of which are: (i) the need to reach a consensus regarding optimal image analysis, (ii) the need to assess the effect of measurement variation caused by using different smartphones and (iii) the need to standardize validation procedures to obtain robust data. Addressing these issues will drive the development of SBDs and potentially unlock their massive potential for citizen-based food control., Highlights • Optical smartphone based sensors in the food safety field are systematically reviewed. • Recommendations on image analysis optimization are given. • The analytical performance of smartphone based sensors is discussed. • Available commercial devises are critically compared.

Carbamates (CMs) and organophosphates (OPs) are widely used pesticides with known neurotoxicity arising from the inhibition of acetylcholinesterase (AChE). When AChE is active, in vitro, it can hydrolyze certain substrates to colored products while in the presence of an inhibitor this color development is decreased. Based on this principle, an AChE assay for CM and OP compounds was optimized and validated for carbofuran, carbofuran-3-hydroxy and dichlorvos in lettuce and strawberry extracts. The analytical performance of the assay was confirmed by an accredited liquid chromatography tandem mass spectrometry (LC&ndash, MS/MS) method. The developed AChE assay achieved low limits of detection (LODs) at the part per billion (ppb) level, depending the analyte inhibitory strength, recovery rates higher than 70% and good repeatability. Moreover, the toxic unit (TU) approach was applied, for extracts containing the validated analytes, and antagonism was noticed in all cases. Overall, the developed method is rapid, simple, cost-effective and may find application as a low-cost pre-screening tool of AChE inhibitors presence. Last but not least, this study can be considered a guide on development, validation and benchmarking of bioassays in food safety, a topic, which is commonly mispresented in the available literature.

Foodstuffs contaminated by mycotoxins have been reported around the globe resulting in significant financial losses and health-threating cases due to dietary exposure. Commonly, two analytical approaches are used in mycotoxin analysis, namely screening bioanalytical methods such as immunoassays and confirmatory chromatographic analysis which are related to certain merits and challenges. In this study, to provide an alternative combining rapidness and unequivocal analyte identification, a direct analysis in real time ion source coupled to orbitrap mass spectrometry (DART-Orbitrap MS) method was developed and validated for the detection of 19 mycotoxins in cereal flour matrices. Excellent detectability expressed as the lowest calibration level (LCL) ranging between 25 μg kg−1 and 250 μg kg−1 depending on the analyte was achieved as well as satisfactory precision and trueness. To identify advantages and drawbacks of the in-house DART-Orbitrap MS method against the golden standard methods, a critical comparison towards liquid chromatography (LC) coupled to high and low resolution MS was performed. DART-Orbitrap MS high throughput and rapidity was revealed while LC-MS proved its superior detectability, which is of indispensable importance for mycotoxin regulatory control. In conclusion, the developed DART-Orbitrap MS method can be applied to intensify and accelerate the monitoring of specific mycotoxins in cereal matrices.

It is less than 20 years since nanotechnology found applications in food packaging. The new packaging materials have featured various improved characteristics such as antimicrobial activity and active packaging. However, there is a great controversy about the production cost, safety and suitability of nanocomposite materials to come in contact with foodstuffs. To this end, we critically summarize the literature in order to provide the overview of the current status in the field. A scientometric evaluation is presented for the first time in order to illustrate the state of the art. The USA and the Asian countries are the leaders, while the EU countries follow. Additionally, as the analysis of nanomaterials in food matrices is still in early stage, there is an emerging demand to review the analytical techniques which are capable for the monitoring of nanomaterials. Microscopy, spectroscopy, separation and mass spectrometry techniques show advantages and drawbacks which are discussed. FFF-ICP-MS and sp-ICP-MS have the greatest potential for the detection of inorganic nanoparticles in food. In conclusion, the difficulty of analyzing nanoparticles is increased by the lack of standard solutions, reference materials, standard methods and the limited number of available inter-laboratory proficiency tests.

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&ndash, 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.

Food contaminants monitoring is conducted in an intensive manner yet, there are still food safety scandals related to various chemical compounds. This fact highlights the need to review the requirements posed by the current legal framework on analytical methods performance and evaluate its application in published studies. Herein, we present an inventory including more than 470 publications on screening and confirmatory methods, which were used to control hazardous compounds such as pesticides, antibiotics, mycotoxins, aquatic toxins and allergens. Analytical performance characteristics, trends and state of the art, both merits and shortcomings, are critically discussed and summarized in excel tabulations. This repository highlights the ever-increasing use of screening methods and the necessity to confirm their performance by applying confirmatory methods. In conclusion, more effort is needed on validation and benchmarking, especially of newly developed technology such as smartphone-based methods, to avoid false-negative results and ensure that methods fit for purpose. © 2019 The Authors, This project has received funding from the European Union's Horizon 2020 research and innovation program under the Marie Sklodowska-Curie grant agreement No 720325 , FoodSmartphone. Appendix A

Acute intoxication incidents due to neurotoxic organophosphate (OP) insecticides are occasionally reported, related either to suicidal attempts or occupational exposure due to the misuse of protective equipment. Among them, chlorpyrifos is a compound related to great controversy, which is still authorized and easily accessible in many countries around the world. However, to screen for its exposure markers, instrumental methods are commonly applied, which cannot enable rapid monitoring at an early stage of an intoxication. Therefore, in this study, a microfluidic paper-based analytical device (mu PAD) able to rapidly screen for chlorpyrifos-oxon, the toxic chlorpyrifos metabolite, in human serum was developed and fully validated. The mu PAD combines wax-printed butyrylcholinesterase (BChE) paper sensors, a lab-on-a-chip (LOC) prototype injector and a smartphone as the analytical detector. In principle, the wax-printed strips with adsorbed BChE are embedded into LOC injectors able to deliver samples and reagents on-demand. A smartphone reader was used to monitor the color development on the strips providing binary qualitative results. mu PAD method performance characteristics were thoroughly evaluated in terms of specificity, detection capability (CC beta) and ruggedness. The developed analytical platform is rapid (results within 10 min), cost-efficient (0.70 (sic)), potentially applicable at the point-of-need and attained a low CC beta (10 mu g L-1 in human serum). Finally, mu PAD characteristics were critically compared to wellestablished methods, namely an in-house BChE microplate assay and liquid chromatography tandem mass spectrometry. Funding Agencies|European Unions Horizon 2020 research and innovation program under the Marie Sklodowska-Curie grantEuropean Union (EU) [720325]; METROFOOD-CZ research infrastructure project (MEYS Grant) [LM2018100]; [A2_FPBT_2020_013]

Greek Protected Designation of Origin (PDO) cheeses are characterised by high nutritional values and origin traits. The aim of the study was to determine the content of 65 elements, of Greek PDO cheeses, through inductively coupled plasma-mass spectrometry and examine the elemental metabolome as a potential authenticity marker. One hundred twelve samples from 21 PDO, one potential PDO and nine non-PDO cheeses were assessed. Discriminant analysis based on total fingerprinting was able to determine the geographic origin with 99.1% accuracy. The most significant variables of the model were Ce, Dy, Eu, Gd, Ho, La, Nd, Pr, Sm, Tb, Y, Yb, Pd, As, Ba, Co, Fe, Ga, Mo, Ni, Ti, Zr, Ca and P. The results demonstrate that elemental metabolomics can be successfully applied for cheese authentication. The elemental fingerprint could provide a reliable discrimination while rare earth elements are promising authenticity markers.

Detailed knowledge regarding sensor based technologies for the detection of food contamination often remains concealed within scientific journals or divided between numerous commercial kits which prevents optimal connectivity between companies and end-users. To overcome this barrier The End user Sensor Tree (TEST) has been developed. TEST is a comprehensive, interactive platform including over 900 sensor based methods, retrieved from the scientific literature and commercial market, for aquatic-toxins, mycotoxins, pesticides and microorganism detection. Key analytical parameters are recorded in excel files while a novel classification system is used which provides, tailor-made, experts’ feedback using an online decision tree and database introduced here. Additionally, a critical comparison of reviewed sensors is presented alongside a global perspective on research pioneers and commercially available products. The lack of commercial uptake of the academically popular electrochemical and nanomaterial based sensors, as well as multiplexing platforms became very apparent and reasons for this anomaly are discussed.