A critical comparison between an ultra-high-performance liquid chromatography triple quadrupole mass spectrometry (UHPLC-QqQ-MS) method and an enzyme assay for anti-cholinesterase pesticide residue detection in cereal matrices.

Analytical method development for the control of pesticide residues occurring in significant dietary foodstuffs is of utmost importance considering their potential impact on consumer health and food market sustainability. Depending on the purpose, either instrumental analysis, mainly chromatographic methods, or screening assays, mostly using biorecognition affinity, are commonly used, featuring different advantages and drawbacks. To practically compare these two different types of analytical strategies, we applied them for the detection of (i) 97 organophosphate (OP) and carbamate (CM) pesticide residues in wheat flour and (ii) carbofuran (a carbamate insecticide) in wheat, rye and maize flour samples. Regarding high-end analysis, an ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ-MS) method was developed and validated achieving low limits of quantification (LOQs, from 0.002 to 0.040 mg kg-1) and a short chromatographic run (12 min). In terms of bioanalytical methods, a fast (17 min) and cost-efficient (∼0.01€ per sample) acetylcholinesterase (AChE) microplate assay for carbofuran screening was utilized. Importantly, carbofuran was the strongest of the 11 OP and CM tested pesticides achieving a half maximal inhibitory concentration (IC50) of 0.021 µM whilst the assay detectability was at the parts per billion level in all three cereal matrices. Based on the attained results, a critical discussion is presented providing the analytical merits and bottlenecks for each case and a wider outlook related to the application of analytical methods in the food safety control analytical scheme.

A microfluidic paper-based analytical device (µPAD) with smartphone readout for chlorpyrifos-oxon screening in human serum.

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 (µPAD) able to rapidly screen for chlorpyrifos-oxon, the toxic chlorpyrifos metabolite, in human serum was developed and fully validated. The µPAD 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. µPAD method performance characteristics were thoroughly evaluated in terms of specificity, detection capability (CCß) and ruggedness. The developed analytical platform is rapid (results within 10 min), cost-efficient (0.70 €), potentially applicable at the point-of-need and attained a low CCß (10 µg L-1 in human serum). Finally, µPAD characteristics were critically compared to well-established methods, namely an in-house BChE microplate assay and liquid chromatography tandem mass spectrometry.

Smartphone-based optical assays in the food safety field.

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.

Tissue distribution of rare earth elements in wild, commercial and backyard rabbits.

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.

The end user sensor tree: An end-user friendly sensor database.

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.