Ochratoxin A (OTA) is one of the most important dietary risk factors and is classified as a possible carcinogen to humans. Assessing the conditions to remove it from foodstuffs in a simple and effective way is of the utmost importance. OTA behaviour in water in the pH range 1.0–12.5 was elucidated to investigate the conditions for irreversible toxicity inactivation of OTA. The results indicate that four forms, from neutral to trianionic, intervene depending on the pH. pKa1,2 were rigorously established by independent spectroscopic techniques to overcome the scarcity of literature. Then, Density Functional Theory (DFT) calculations were used to determine the most probable degradation mechanism and this was confirmed by fluorescence spectroscopy. At pH 12.5, hydrolyzation of the lactone ring starts in less than one hour, but only after two hours does the degradation process lead to fragmentation. After one week this process is not yet completed. The reaction products occurring upon re-acidification were also investigated. OTA degradation is still reversible if acidic conditions are promptly restored, yielding again a hazardous molecule. However, degradation becomes irreversible after fragmentation. This finding suggests proceeding with due caution if a base is exploited to remove the toxin.
15 January 2013 in IEEE Transactions on Instrumentation and Measurement
Conductivity measurements of liquids ask for measurements of impedance spectra in a wide frequency range to identify stray parameters caused by electrode-surface effects. On low-conductivity liquids, such as ultrapure water, frequencies of interest range below those available on precision $LCR$ meter (usually in the 10-Hz range). A new impedance spectrometer based on multifrequency excitation and discrete Fourier transform analysis is presented here. The spectrometer defines the impedance under measurement as a two-port standard and measures impedance spectra covering 5 dec, reaching frequencies in the millihertz range. The instrument accuracy is verified by measurements on calibrated resistance standards. As an example of application, measurement results on pure-water samples and a comparison with measurements performed with an $LCR$ meter are reported.
Monitoring the state of oceans and their evolution in space and time is of fundamental importance as they are severely impacted by climate change, showing an increase in temperature, acidity and stratification. The role of metrology in the marine sector is relevant for helping oceanographers consolidate measurement approaches already in place by introducing concepts like metrological traceability and measurement uncertainty. The aim of this paper is to present some examples of successful and potential applications of metrology in oceanographic research, with a focus on past and ongoing activities in the framework of joint research cooperation, which could be applied by oceanographers to consolidate the comparability of data acquired in different experimental conditions, and places and time for some essential ocean variables. Scientific cooperation in the framework of joint research projects is particularly useful for supporting measurement capabilities in marine research worldwide, and the technologies and methods developed so far represent a starting point for improvements in international monitoring networks. These techniques may be applied by laboratories and centres working in the marine sector. Applications and possible future developments will also be discussed in this paper.
A simple procedure for field fish sample pretreatment was developed. This treatment in combination with square wave anodic stripping voltammetry (SW-ASV) with solid gold electrodes (SGE) and gold nanoparticle-modified glassy carbon electrodes (AuNPs-GCE) was applied for the determination of total mercury content. A certified reference material (CRM, Tuna Fish BCR 463), ten freeze-dried samples of canned tuna and two fresh fish samples were analysed both with a bench-top voltammetric analyser after microwave digestion and with a portable potentiostat after mild eating using a small commercial food warmer. The results obtained by the two SW-ASV approaches and by a Direct Mercury Analyser (DMA), the official method for mercury determination, were in very good agreement. In particular, (i) the results obtained with in field procedure are consistent with those obtained with the conventional microwave digestion; (ii) the presence of gold nanoparticles on the active electrode surface permits an improvement of the analytical performance in comparison to the SGE: the Limit of Quantification (LOQ) for mercury in fish-matrix was 0.1 μg L−1 (Hg cell concentration), corresponding to 0.06 mg kg−1 wet fish, which is a performance comparable to that of DMA. The pretreatment proposed in this study is very easy and applicable to fresh fish; in combination with a portable potentiostat, it proved to be an interesting procedure for on-site mercury determination.
Purity analysis of parent gases used to produce reference gas mixtures is fundamental to assure the metrological traceability of the certified gas composition, and the use of purity data in the calculation of the mixture composition should be performed in accordance with the requirements of international standards. Purity analysis can be difficult to realize since limited measurement standards are available for the determination of trace levels of gaseous compounds. The first step of purity analysis is the definition of the impurities considered critical or significant to the final composition of a mixture. In this work, we present the activity carried out for the identification and quantification of impurities of carbon dioxide and water in some ultrapure gases used for the preparation of primary certified reference gas mixtures of carbon dioxide at atmospheric amount fraction (400–800 µmol·mol−1), by means of different spectroscopic techniques (Fourier Transform IR, Non-Dispersive IR and Cavity Ring-Down). Dynamic dilution was used for the generation of reference mixtures for the calibration of the analyzers by using calibrated Mass Flow Controllers. The certified reference gas mixtures produced with the tested pure gases will also be applied to characterization studies and calibration protocols for gas sensors used both for outdoor and indoor monitoring.