Search Results (38)

An LC–Orbitrap–HRMS method was developed and validated for the simultaneous determination of four tetracyclines—oxytetracycline (OTC), tetracycline (TC), doxycycline (DC), and chlortetracycline (CTC)—in milk. This method involves sample extraction with McIlvaine–EDTA buffer solution (pH 4) and solid-phase extraction (SPE) with Oasis HLB cartridges, followed by the evaporation of the extract and its reconstitution with a 14% methanol aqueous solution before injection into the instrumental system. This method has been validated in terms of linearity, sensitivity, selectivity, precision, and accuracy, in accordance with Commission Decision 2002/657/EC requirements. Compared to existing methods, this approach optimally combines a quantitative procedure for extracting analytes from the milk of different species, including sheep, bovines, and goats, with a very short LC–Orbitrap–HRMS instrumental analysis time (only 8 min), simultaneously ensuring high precision, sensitivity, and applicability as a rapid confirmation method in official food control laboratories. The proposed method was applied to determine the concentration levels of OTC in milk samples derived from healthy Sardinian sheep and those naturally infected with Streptococcus uberis, after the intramuscular administration of an antibiotic, in order to evaluate how much of the drug was “subtracted” during penetration from blood into milk, with a potential effect of reducing its therapeutic efficacy. Full article

The African Swine Fever Virus (ASFV) is a DNA virus of the Asfarviridae family, Asfivirus genus. It is responsible for massive losses in pig populations and drastic direct and indirect economic impacts. The ever-growing handling of ASFV pathological material in laboratories, necessary for either diagnostic or research activities, requires particular attention to avoid accidental virus release from laboratories and its detrimental economic and environmental effects. Recently, the Commission Delegated Regulation (EU) 2020/689 of 17 December 2019 repealed the Commission Decision of 26 May 2003 reporting an ASF diagnostic manual (2003/422/EC) with the minimum and supplementary requirements for ASF laboratories. This decision generated a regulatory gap that has not been addressed yet. This paper aims to describe the Italian National Reference Laboratory (NRL) efforts to develop an effective and reliable biological containment tool for ASF laboratories and animal facilities. The tool consists of comprehensive and harmonized structural and procedural requirements for ASF laboratories and animal facilities that have been developed based on both current and repealed legislation, further entailing a risk assessment and internal audit as indispensable tools to design, adjust, and improve biological containment measures. Full article

A profile of the microbial safety and hygiene of cheese in central Italy was defined based on an analysis of 1373 cheeses sampled under the Italian National Control Plan for Food Safety spanning the years 2013 to 2020 and tested according to Commission Regulation (EC) No. 2073/2005 (as amended). A total of 97.4% of cheese samples were assessed as being satisfactory for food safety criteria and 80.5% for process hygiene criteria. Staphylococcal enterotoxin was found in 2/414 samples, while Salmonella spp. and Listeria monocytogenes were detected in 15 samples out of 373 and 437, respectively. Escherichia coli and coagulase-positive staphylococci counts were found unsatisfactory in 12/61 and 17/88 cheese samples, respectively. The impact of milking species, milk thermal treatment, and cheese hardness category was considered. A statistically significant association (p < 0.05) was found between milk thermal treatment and the prevalence of coagulase-positive staphylococci and Listeria monocytogenes and between hardness and unsatisfactory levels of Escherichia coli. The data depict a contained public health risk associated with these products and confirm, at the same time, the importance of strict compliance with good hygiene practices during milk and cheese production. These results can assist in bolstering risk analysis and providing insights for food safety decision making. Full article

Urban areas constitute one of the main issues of sustainability as defined by the United Nations with the Sustainable Development Goals (SDGs). The recent smart city concept represents a way for achieving the urban sustainability goals. The European Commission (EC) bases the smart city concept on three pillars: energy, transport and Information and Communication Technologies (ICT). The main objective of the paper is to investigate the European smart city process, by focusing on urban mobility and their interconnections with the other two pillars. The methodological approach of territorial planning is used by identifying the plan dimensions and then analyzing the processes at master and sectorial level. The applied processes are verified with a review of the European documents that constitute the rules for defining and implementing the smart city concept. European guidelines indicate the SUMP as the integrated master plan that contributes to reach the convergence among energy, transport and ICT processes. By focusing on people mobility sector, European cities are implementing the Mobility as a Service (MaaS) plan at the sectorial level. This implies the necessity to enhance the knowledge of mobility phenomenon, in relation to emerging ICT and their impact on energy consumptions. The contribution of the work is given by the identification of a planning and implementation path focused on smart city, in urban areas, which connects the general goals of Agenda 2030 with the daily implications for citizens and therefore with the specific results. The paper results are useful: from one side, for researchers that work on advancements of theories, and from another side, for planners and decision makers to explore the European attempts towards urban sustainability and the real implementations on urban mobility systems. Full article

A quantitative and qualitative method using a high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) detection approach was developed and validated for the analysis of tigecycline, four tetracyclines and their three 4-epimer derivatives in chicken muscle. Samples were extracted repeatedly with 0.1 mol/L Na₂EDTA–McIlvaine buffer solution. After vortexing, centrifugation, solid-phase extraction, evaporation and reconstitution, the aliquots were separated using a C8 reversed-phase column (50 mm × 2.1 mm, 5 µm) with a binary solvent system consisting of methanol and 0.01 mol/L trichloroacetic acid aqueous solution. The typical validation parameters were evaluated in accordance with the acceptance criteria detailed in the guidelines of the EU Commission Decision 2002/657/EC and the U.S. Food and Drug Administration Bioanalytical Method Validation 05/24/18. The matrix-matched calibration curve was linear over the concentration range from the limit of quantitation (LOQ) to 400 μg/kg for doxycycline, and the calibration graphs for tetracycline, chlortetracycline, oxytetracycline, their 4-epimer derivatives and tigecycline showed a good linear relationship within the concentration range from the LOQ to 200 μg/kg. The limits of detection (LODs) for the eight targets were in the range of 0.06 to 0.09 μg/kg, and the recoveries from the fortified blank samples were in the range of 89% to 98%. The within-run precision and between-run precision, which were expressed as the relative standard deviations, were less than 5.0% and 6.9%, respectively. The applicability was successfully demonstrated through the determination of residues in 72 commercial chicken samples purchased from different sources. This approach provides a novel option for the detection of residues in animal-derived food safety monitoring. Full article

This study developed and validated an analytical methodology for the determination of aflatoxins, enniatins, beauvericin, zearalenone, ochratoxin-A, alternariols, HT-2 and T-2 toxin in soy, oat, rice and almond beverages, based on solid phase extraction columns (SPE) and analyzed by liquid chromatography coupled to mass spectrometry in tandem. C18 SPE was successfully applied, obtaining recoveries that range from 72 ± 12% (ochratoxin-A) to 99 ± 4% (ENA1) at high level (L1) and 65 ± 8% (T-2) to 128 ± 9% (alternariol monomethyl ether) at low levels (L3). The methodology was validated according to Commission Decision 2002/657/EC, with limits of quantification ranging from 0.3 (AFs in oat beverages) to 18 ng/mL (HT-2 in rice beverage). The analysis of 56 beverage samples purchased from Valencia (Spain) showed at least one mycotoxin occurring in 95% of samples, including carcinogenic aflatoxins, and oat beverage was the most contaminated. This is a newest validated methodology for the quantification of sixty mycotoxins in oat, rice, almond and soy beverages. Full article

Antibacterial substances such as sulfonamides are widely used in veterinary medicine to treat many bacterial diseases. After their administration to animals, up to 90% of the initial dose of the antibiotic is excreted in the feces and/or urine, which can be applied to farmland as natural or organic fertilizers. In this work, an analytical method was developed with the use of HPLC-FLD for the detection and quantification of five sulfonamides (sulfaguanidine, sulfadiazine, sulfamerazine, sulamethazine and sulfamethoxazol) in poultry and pig feces, slurry and digestates. The method was validated according to EU requirements (Commission Decision 2002/657/EC and VICH GL49). Linearity, decision limit, detection capability, detection and quantification limits, recovery, precision, and selectivity were determined, and adequate results were obtained. Using the HPLC-FLD method for all analyzed matrices, recoveries were satisfactory (77.00–121.16%), with repeatability and reproducibility in the range of 4.36–17.34% to 7.94–18.55%, respectively. Decision limit (CCα) and detection capability (CCβ) were 33.87–67.63 and 53.36–92.00 µg/kg, respectively, and limit of detection (LOD) and limit of quantification (LOQ) were 13.53–23.30 and 26.02–40.38 µg/kg, respectively, depending on the analyte. The forty-four samples of natural and organic fertilizers were analyzed, and four samples showed sulfamethoxazole in the amount from range 158 to 11,070 µg/kg. The application of antibiotics including sulfonamides for farming animals is widespread and may lead to the development of antibiotic resistance and other environmental effects. Full article

The presented procedure combines experience from two LC-MS/MS methods previously developed by our team for NSAIDs determination in meat and milk. The novelty was a modification of sample preparation and combining LC-MS/MS method for milk and muscle. The clean-up procedure was investigated, leading to a change from SPE to dSPE with C18 bulk sorbent. Unlike most of the existing methods, chromatographic separation was achieved on a C8 chromatographic column. This method was developed and validated under European Commission Decision 2002/657/EC. Recovery for milk samples values between 86.3% to 108%, with the coefficient of variation, varied from 5.51% to 16.2%. The recovery for muscle was calculated to be between 85.0% and 109%, and the coefficient of variation was—4.73% to 16.6%. The validation results prove that the method is suitable for confirmatory purposes in milk and muscle. Of 452 samples tested in 2019 and 2020, two have been identified as non-compliant. Full article

Sand mining is one of the major sustainability challenges of the 21st century. Rates of extraction are surpassing sand supply, and ensuing sand starvation is adversely impacting channel-floodplains and deltas. Therefore, quantifying sand mining’s location and extent, through global monitoring and detection, particularly in fluvial systems, is becoming a priority. Sand mining by dredges and barges (extraction of sand and secondarily gravel) in South East Asian rivers, including illegal sand mining, has become rampant, and a monitoring system is not yet in place. Here, we present a high-resolution remote sensing-based mining monitoring system for sand mining in fluvial systems. We used Sentinel-1 mission, a radar component of the Copernicus joint initiative of the European Commission (EC) and the European Space Agency (ESA). The system, tested in the Ayeyarwady, the second largest river in SE Asia, detects sand mining by barges almost in real-time with a satisfactory accuracy level. An additional advantage of the monitoring system is that it does not incur any costs, making it accessible to multiple users, decision-makers, and stakeholders. Full article

An ultra-high performance liquid chromatography tandem mass spectrometry method was developed and validated for the sensitive determination and unambiguous confirmation of residues of per and polyfluorinated alkyl substances (PFAS) in breastmilk, retail milk and infant formulas following two sample preparation methods. Sample pre-treatment was carried out by a simplified QuEChERS method without requiring dSPE or any further clean-up. The method was validated in accordance with the requirements of Commission Decision 657/2002/EC with slight modifications. The method displayed good linearity with R² ranging from 0.9843–0.9998 for all target PFAS. The recovery and within-laboratory reproducibility of the method (n = 63) were in the range 60–121% and 5–28%, respectively. The decision limit, detection capability and limit of quantitation ranged from 30–60 ng kg⁻¹ to 40–100 ng kg⁻¹ and 5–50 ng kg⁻¹, respectively. Acceptable matrix effect values in the range −45–29% were obtained with uncertainty of measurement lower than 25% for all target PFAS. The method displays its suitability for the sensitive and high-throughput confirmatory analysis of C₄–C₁₄ PFAS in breastmilk, dairy milk and infant formulas. Full article

Biomonitoring of biological samples arises as an effective tool to evaluate the exposure to mycotoxins in the population. Owing to the wide range of advantages, there is a growing interest in the use of non- and minimally invasive alternative sampling strategies, such as dried blood spot sampling or volumetric absorptive microsampling (VAMS). A VAMS-based multi-mycotoxin method was developed and validated for 24 different mycotoxins. Method validation was based on the Bioanalytical Method Validation Guideline of the Food and Drug Administration from the United States and for most of the studied mycotoxins, the results of the performance characteristics were in agreement with the criteria of the European Commission Decision 2002/657/EC. The recovery for the different mycotoxins was not haematocrit dependent and remained acceptable after storing the VAMS for 7 and 21 days at refrigeration temperature (4 °C) and room temperature, demonstrating that VAMS could be applied to assess mycotoxin exposure in blood in resource-limited areas, where there may be a delay between sampling and analysis. Finally, a comparison between VAMS and a procedure for liquid whole blood analysis, performed on 20 different blood samples, did not result in missed exposed cases for VAMS. Moreover, both methods detected similar levels of ochratoxin A, ochratoxin alpha, zearalenone and aflatoxin B1. Given all the benefits associated with VAMS and the developed method, VAMS sampling may serve as an alternative to conventional venous sampling to evaluate multiple mycotoxin exposure. Full article

Colistin, an imperative member of the polymyxin group, is a cationic peptide antibiotic. Itis also known as polymyxin E, but this peptide antibiotic has been forbidden for human consumption due to its high toxicity. Regrettably, this antibiotic is utilized as a feed additive and veterinary drug for animals. Due to the toxicity of colistin, the presence of its residue in the animal system represents a threat to human health regarding the consumption of meat, especially chicken. A novel method was proposed for quantifying colistin B in chicken muscles and eggs using ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). In this method, extraction of colistin B from samples was achieved by mixing the sample with acidified methanol:water (1/1, v/v), followed by centrifugation and filtration by a membrane filter excluding solid-phase extraction (SPE) clean up, as well as evaporation steps. The analysis was conducted by optimized liquid chromatography–tandem mass spectrometry (LC–MS/MS), and method performance was assessed in terms of the limit of quantitation, specificity, selectivity, precision, linearity and recovery in coherence with the guidelines of SANTE and the Commission Decision 2002/657/EC. The result obtained from the study showed the limit of quantitation (LOQ) as 10 µg Kg⁻¹ for muscles and 5 µg Kg⁻¹ for eggs, with acceptable recoveries along with precision. The linearity was plotted in the range of 5–25 µg L⁻¹ (solvent) for egg and 10–50 µg Kg⁻¹ (matrix-matched) for muscles. The result of average recoveries showed the value of 70–94% (3.3–12% relative standard deviation (RSD)) for chicken muscles and 88–107% (2.5–18.6% RSD) for egg samples, which meets the criteria for acceptability of method according to both SANTE and 2002/657/EC guidelines. This proposed protocol provides a cost-effective solution for food testing labs by reducing the cost of the sample preparation by 60% along with the time required for SPE cleanup. Further, the optimized method was also tested on real samples collected from nearby provinces in Solan city, Himachal Pradesh, India, and three out of 20 muscles were found to have colistin B in the range of 50–560 µg Kg⁻¹. Full article

In this work, for the first time, Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry (UHPLC–MS/MS) method was developed for qualitative and quantitative analysis of veterinary antibiotics (cephalosporins, diaminopyrimidines, fluoro(quinolones), lincosamides, macrolides, penicillins, pleuromutilins, sulfonamides, tetracyclines, and sulfones) in hen eggshells. The sample preparation method is based on a liquid–liquid extraction with a mixture of metaphosphoric acid, ascorbic acid, EDTA disodium salt dihydrate, and acetonitrile. The chromatographic separation was performed on Luna^® Omega Polar C18 10 column in gradient elution mode and quantitated in an 8 min run. Validation such as linearity, selectivity, precision, recovery, matrix effect, limit of quantification (LOQ), and limit of detection (LOD) was found to be within the acceptance criteria of the validation guidelines of the Commission Decision 2002/657/EC and EUR 28099 EN. Average recoveries ranged from 81–120%. The calculated LOQ values ranged from 1 to 10 µg/kg, the LOD values ranged from 0.3 to 4.0 µg/kg, depending on analyte. The developed method has been successfully applied to the determination of antibacterial compounds in hen eggshell samples obtained from different sources. The results revealed that enrofloxacin, lincomycin, doxycycline, and oxytetracycline were detected in hen eggshell samples. Full article

Situational awareness refers to the process of aggregating spatio-temporal variables and measurements from different sources, aiming to improve the semantic outcome. Remote Sensing satellites for Earth Observation acquire key variables that, when properly aggregated, can provide precious insights about the observed area. This article introduces a novel automatic system to monitor the activity levels and the operability of large infrastructures from satellite data. We integrate multiple data sources acquired by different spaceborne sensors, such as Sentinel-1 Synthetic Aperture Radar (SAR) time series, Sentinel-2 multispectral data, and Pleiades Very-High-Resolution (VHR) optical data. The proposed methodology exploits the synergy between these sensors for extracting, at the same time, quantitative and qualitative results. We focus on generating semantic results, providing situational awareness, and decision-ready insights. We developed this methodology for the COVID-19 Custom Script Contest, a remote hackathon funded by the European Space Agency (ESA) and the European Commission (EC), whose aim was to promote remote sensing techniques to monitor environmental factors consecutive to the spread of the Coronavirus disease. This work focuses on the Rome–Fiumicino International Airport case study, an environment significantly affected by the COVID-19 crisis. The resulting product is a unique description of the airport’s area utilization before and after the air traffic restrictions imposed between March and May 2020, during Italy’s first lockdown. Experimental results confirm that the proposed algorithm provides remarkable insights for supporting an effective decision-making process. We provide results about the airport’s operability by retrieving temporal changes at high spatial and temporal resolutions, together with the airplane count and localization for the same period in 2019 and 2020. On the one hand, we detected an evident change of the activity levels on those airport areas typically designated for passenger transportation, e.g., the one close to the gates. On the other hand, we observed an intensification of the activity levels over areas usually assigned to landside operations, e.g., the one close to the hangar. Analogously, the airplane count and localization have shown a redistribution of the airplanes over the whole airport. New parking slots have been identified as well as the areas that have been dismissed. Eventually, by combining the results from different sensors, we could affirm that different airport surface areas have changed their functionality and give a non-expert interpretation about areas’ usage. Full article

Nitrogen dioxide (NO₂) is one of the main air quality pollutants of concern in many urban and industrial areas worldwide, and particularly in the European region, where in 2017 almost 20 countries exceeded the NO₂ annual limit values imposed by the European Commission Directive 2008/50/EC (EEA, 2019). NO₂ pollution monitoring and regulation is a necessary task to help decision makers to search for a sustainable solution for environmental quality and population health status improvement. In this study, we propose a comparative analysis of the tropospheric NO₂ column spatial configuration over Europe between similar periods in 2019 and 2020, based on the ESA Copernicus Sentinel-5P products. The results highlight the NO₂ pollution dynamics over the abrupt transition from a normal condition situation to the COVID-19 outbreak context, characterized by a short-time decrease of traffic intensities and industrial activities, revealing remarkable tropospheric NO₂ column number density decreases even of 85% in some of the European big cities. The validation approach of the satellite-derived data, based on a cross-correlation analysis with independent data from ground-based observations, provided encouraging values of the correlation coefficients (R²), ranging between 0.5 and 0.75 in different locations. The remarkable decrease of NO₂ pollution over Europe during the COVID-19 lockdown is highlighted by S-5P products and confirmed by the Industrial Production Index and air traffic volumes. Full article