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Food authentication, including the differentiation of geographical or botanical origin, the method of production i.e. organic vs. conventional farming as well as the detection of food fraud/adulteration, has been a rapidly growing field over the past two decades due to increasing public awareness regarding food quality and safety, nutrition, and health. Concerned parties include consumers, producers, and legislators. Thus, the development of rapid, accurate, sensitive, and reproducible analytical methods to guarantee the authenticity of foods is of primary interest to scientists and technologists. The aim of the present article is to summarize research work carried out on the authentication of Greek agricultural products using spectroscopic (NIR, FTIR, UV-Vis, Raman and fluorescence spectroscopy, NMR, IRMS, ICP-OES, ICP-MS) and chromatographic (GC, GC/MS, HPLC, HPLC/MS, etc.) methods of analysis in combination with chemometrics highlighting the chemical markers that enable product authentication. The review identified a large number of chemical markers including volatiles, phenolic substances, natural pigments, elements, isotopes, etc. which can be used for (i) the differentiation of botanical/geographical origin; conventional from organic farming; production procedure and vintage year, etc. and (ii) detection of adulteration of high quality plant and animal origin foods with lower value substitutes. Finally, the constant development of reliable analytical techniques in combination with law enforcement authorities will ensure authentic foods in terms of quality and safety for consumers., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

A quantitative analytical procedure was developed and validated by the use of Ultra- Performance Liquid Chromatography tandem Mass Spectrometry (UPLC-MS/MS) for the determination of Cannabidiol (CBD), Cannabinol (CBN), Δ 9 -Tetrahydrocannabinol (Δ 9 -THC), Cannabichromene (CBC), Cannabigerol (CBG) and 11-Nor- 9- Carboxy- Tetrahydrocannabinol (THC-COOH) in an unconventional biological matrix, cerumen. All the investigated calibration curves were characterized by high correlation values (R 2 ≥ 0.9965). The LODs and LOQs ranged from 0.004 to 0.009 μg g -1 and 0.012-0.029 μg g -1 , respectively. Intra-assay and inter-assay precision were found to be 0.6-2.5%, and 0.8-2.2%, respectively. All recovery values of cannabinoids, with the use of the optimum cotton swab, at low (0.008 μg g -1 of cerumen), medium (0.037 μg g -1 of cerumen) and high (0.16 μg g -1 of cerumen) control levels, were estimated to be above 86%. The method developed here permitted the analysis of real cerumen samples obtained from fourteen cannabis users. In twelve out of fourteen cases, Δ 9 -THC was found to be positive, while in six cases, three major cannabinoids, CBN, CBG and Δ 9 -THC were quantified at concentrations 0.02-0.21 μg g -1 , 0.01-0.24 μg g -1 and 0.01-4.86 μg g -1 , respectively. Subject #8 has the highest amount of the detected substances in both left and right ear, with Δ 9 -THC at a concentration of 1.85 and 4.86 μg g -1 , CBG 0.06 and 0.24 μg g -1 , CBN 0.10 and 0.21 μg g -1 , respectively. In addition, a detection window for the substances Δ 9 -Tetrahydrocannabinol, Cannabinol and Cannabigerol, in cerumen, was defined with success. In this case, Δ 9 -THC reached a maximum detection frame of up to fifteen days after smoking 0.5 g of marijuana cigarette. ANOVA-one-way analysis also indicated that the average earwax production of non-cannabis users differs significantly from the one of cannabis users (p = 0.048, <0.05). On the other hand, no significant difference was noticed between male and female users as the p value exceeded 0.05. In addition, no significant effect was observed on earwax production in regard to age, frequency and the last time of use (p > 0.05). These last three factors proved to have a significant impact on cannabinoids concentrations, since p values were less than 0.05., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

In this study, cerumen, a non-conventional biological secretion, was examined as an alternative matrix for forensic analyzis. A fully validated analytical UPLC-MS/MS method was developed for the detection and quantification of the most prevalent psychoactive illicit drug globe wide, Δ 9 -tethrahydrocannabinol, commonly known as THC, and four major cannabinoids found in cannabis Sativa. The method was validated, and standard external calibration curves were established with correlation coefficients > 0.99. A validated experimental procedure, along with a direct extraction of cannabinoids with acidified acetonitrile resulted in a short total analyzis time and a good extraction efficiency for all the analytes under study. LOD and LOQ values were determined to be 0.01-0.08 pg/mg and 0.04-0.23 pg/mg, respectively. To prove applicability of the proposed assay, volunteers were selected, and cerumen samples were examined for cannabis. The analyzis by use of UPLC-MS/MS indicated that all samples were positive, reporting recent cannabis abuse. Surprisingly, both THC and Cannabinol (CBN) were detected, and quantification was possible in 75% of the cases., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Seventy-eight graviera cheese samples produced in five different regions of Greece were characterized and discriminated according to geographical origin. For the above purpose, pH, titratable acidity (TA), NaCl, proteins, fat on a dry weight basis, ash, fatty acid composition, volatile compounds, and minerals were determined. Both multivariate analysis of variance (MANOVA) and linear discriminant analysis (LDA) were applied to experimental data to achieve sample geographical discrimination. The results showed that the combination of fatty acid composition plus minerals provided a correct classification rate of 89.7%. The value for the combination of fatty acid compositions plus conventional quality parameters was 94.9% and for the combination of minerals plus conventional quality parameters was 97.4%. When cheeses of the above five geographical origins were combined with previously studied graviera cheeses from six other geographical origins collected during the same seasons in Greece, the respective values for the discrimination of geographical origin of all eleven origins were 89.3% for conventional quality parameters plus minerals; 94.0% for conventional quality parameters plus fatty acids; 94.1% for minerals plus fatty acids; and 95.2% for conventional quality parameters plus minerals plus fatty acids. Such high correct classification rates demonstrate the robustness of the developed statistical model.

Asfaka, fir, flower, forest flowers and orange blossom honeys harvested in the wider area of Hellas by professional beekeepers, were subjected to mineral content analysis using inductively coupled plasma optical emission spectrometry (ICP-OES). The main purpose of this study was to characterize the mineral profile and content of toxic metals such as lead, cadmium and chromium, and investigate whether specific minerals could assist accurately in the botanical origin discrimination with implementation of chemometrics. Twenty-five minerals were identified (Ag, Al, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Si, Ti, Tl, V, Zn) and quantified. Results showed that the mineral content varied significantly ( p < 0.05) according to honey botanical origin, whereas lead, cadmium, and chromium contents ranged between 0.05-0.33 mg kg -1 , <0.05 mg kg -1 , and in the range of <0.12 to 0.39 mg kg -1 , respectively. Fir honeys from Aitoloakarnania region showed the highest mineral content (182.13 ± 71.34 mg kg -1 ), while flower honeys from Samos Island recorded the highest silicon content (16.08 ± 2.94 mg kg -1 ). Implementation of multivariate analysis of variance (MANOVA), factor analysis (FA), linear discriminant analysis (LDA), and stepwise discriminant analysis (SDA) led to the perfect classification (100%) of these honeys according to botanical origin with the use of Al, As, Ca, Mg, Mn, Ni, Pb, Sb, Si, Zn and total mineral content. However, the higher lead content in the majority of samples than the regulated upper limit (0.10 mg kg -1 ), sets the need for further improvements of the beekeepers' practices/strategies for honey production.

Thirty-four honey samples donated by beekeepers and purchased from supermarkets were collected during harvesting years 2010-2014 from Cyprus, Greece, and Egypt. The aims of this study were to characterize honey samples and, if possible, to differentiate honeys according to the honey type on the basis of physicochemical parameter values, mineral content, and their combination using supervised statistical techniques (linear discriminant analysis (LDA)). Physicochemical parameters (colour, pH, free acidity, total dissolved solids, salinity, electrical conductivity, and moisture content) were determined according to official methods, while minerals (Al, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, P, Pb, Sb, Si, Ti, Tl, V, and Zn) using inductively coupled plasma optical emission spectrometry. The majority of honey samples analyzed met the quality criteria set by the European directive and national decision related to honey. Implementation of multivariate analysis of variance (MANOVA) and LDA on specific physicochemical parameters, minerals, or their combination provided a satisfactory classification of honeys according to floral type. The overall correct classification rate (based on the cross-validation method) was 79.4% using 7 minerals and 91.2% using 8 physicochemical parameters. When the 15 parameters were combined, the classification rate of Egyptian honeys was improved by 25%.

The objective of the present study was: i) to characterize Mediterranean citrus honeys based on conventional physicochemical parameter values, volatile compounds, and mineral content ii) to investigate the potential of above parameters to differentiate citrus honeys according to geographical origin using chemometrics. Thus, 37 citrus honey samples were collected during harvesting periods 2013 and 2014 from Greece, Egypt, Morocco, and Spain. Conventional physicochemical and CIELAB colour parameters were determined using official methods of analysis and the Commission Internationale de l' Eclairage recommendations, respectively. Minerals were determined using ICP-OES and volatiles using SPME-GC/MS. Results showed that honey samples analyzed, met the standard quality criteria set by the EU and were successfully classified according to geographical origin. Correct classification rates were 97.3% using 8 physicochemical parameter values, 86.5% using 15 volatile compound data and 83.8% using 13 minerals., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Contamination of shellfish with diarrhetic shellfish poisoning (DSP) toxins readily occurs during algal blooms. Such phenomena raise important public health concerns and thus comprise a constant challenge to shellfish farmers, the seafood industry and health services, considering the increasing occurrence of toxic episodes around the world. To avoid the detrimental effects of such episodes, research has focused on the use of various detoxification methodologies that should be rapid, efficient, easy to apply, and will not alter the quality and sensory properties of shellfish. In the present study, both ozonation (15 mg kg(-1) for 6 h) and γ-irradiation (6 kGy) were utilised in order to reduce the toxin content of contaminated shucked mussels, collected during the DSP episodes of 2007 and 2009 in Greece. DSP toxicity was monitored using the mouse bioassay (MBA) whilst the determination of toxin content of the okadaic acid (OA) group (both free and esterified forms) was carried out by LC/MS/MS analysis. Toxin reduction using γ-irradiation was in the range of 12-36%, 8-53% and 10-41% for free OA, OA esters and total OA, respectively. The appearance and texture of irradiated mussels deteriorated, pointing to a low potential for commercial use of this method. Ozonation of mussels resulted in toxin reduction in the range of 6-100%, 25-83% and 21-66% for free OA, OA esters and total OA, respectively. Reduction of OA content was substantially higher in homogenised mussel tissue compared with that of whole shucked mussels. In addition, differences detected with regard to quality parameters (TBA, sensory attributes) between ozonated and control mussels were not considerable. Even though varying percentage reductions in OA and its derivatives were achieved using ozonation under specific experimental conditions tested, it is postulated that upon optimisation ozonation may have the potential for post-harvest commercial DSP detoxification of shucked mussels., (© 2011 Taylor & Francis)

An approach involving both chemical and biological methods was undertaken for the detection and quantification of the marine toxins okadaic acid (OA), dinophysistoxin-1 (DTX-1) and their respective esters in mussels from different sampling sites in Greece during the period 2006-2007. Samples were analyzed by means of a) high performance liquid chromatography with fluorometric detection (HPLC-FLD), using 9-athryldiazomethane (ADAM), as a pre-column derivatization reagent, b) liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) and c) the mouse bioassay. Free OA and DTX-1 were determined by both HPLC-FLD and LC-MS/MS, while their respective esters were determined only by LC-MS/MS after alkaline hydrolysis of the samples. The detection limit (L.O.D.) and quantification limit (L.O.Q.) of the HPLC-FLD method were 0.015 microg/g HP and 0.050 microg/g HP, respectively, for OA. The detection limit (L.O.D.) and quantification limit (L.O.Q.) of the LC-MS/MS method were 0.045 microg/g HP and 0.135 microg/g HP, respectively, for OA. Comparison of results between the two analytical methods showed excellent agreement (100%), while both HPLC-FLD and LC-MS/MS methods showed an agreement of 97.1% compared to the mouse bioassay., (Copyright 2009 Elsevier Ltd. All rights reserved.)