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Ocean acidification has been broadly recognised to have effects on the structure and functioning of marine benthic communities. The selection of tolerant or vulnerable species can also occur during settlement phases, especially for calcifying organisms which are more vulnerable to low pH–high pCO2 conditions. Here, we use three natural CO2 vents (Castello Aragonese north and south sides, and Vullatura, Ischia, Italy) to assess the effect of a decrease of seawater pH on the settlement of Mollusca in Posidonia oceanica meadows, and to test the possible buffering effect provided by the seagrass. Artificial collectors were installed and collected after 33 days, during April–May 2019, in three different microhabitats within the meadow (canopy, bottom/rhizome level, and dead matte without plant cover), following a pH decreasing gradient from an extremely low pH zone (pH &lt, 7.4), to ambient pH conditions (pH = 8.10). A total of 4659 specimens of Mollusca, belonging to 57 different taxa, were collected. The number of taxa was lower in low and extremely low pH conditions. Reduced mollusc assemblages were reported at the acidified stations, where few taxa accounted for a high number of individuals. Multivariate analyses revealed significant differences in mollusc assemblages among pH conditions, microhabitat, and the interaction of these two factors. Acanthocardia echinata, Alvania lineata, Alvania sp. juv, Eatonina fulgida, Hiatella arctica, Mytilys galloprovincialis, Musculus subpictus, Phorcus sp. juv, and Rissoa variabilis were the species mostly found in low and extremely low pH stations, and were all relatively robust to acidified conditions. Samples placed on the dead matte under acidified conditions at the Vullatura vent showed lower diversity and abundances if compared to canopy and bottom/rhizome samples, suggesting a possible buffering role of the Posidonia on mollusc settlement. Our study provides new evidence of shifts in marine benthic communities due to ocean acidification and evidence of how P. oceanica meadows could mitigate its effects on associated biota in light of future climate change.

Laboratories dealing with the analysis of food of animal origin have to face the shortage of both appropriate certified reference materials and pertinent proficiency tests (PTs). Therefore, internal quality control (IQC) materials have to be prepared in-house. The combination matrix/analytes/concentration, as well as the physical state, is a key issue. The European Union Reference Laboratory for Chemical Elements in Food of Animal Origin (EURL-CEFAO), within its activity as PT provider, has set a procedure to prepare test items of liquid milk spiked with arsenic, cadmium and lead at adequate values of concentration. This work describes in detail the steps of this procedure. Homogeneity and stability of the PT test items thus prepared were evaluated by the EURL-CEFAO using a sensitive and accurate method accredited according to ISO/IEC 17025. The analyte concentrations in spiked milk were found stable up to 18 months which is of particular interest for cadmium due to the low value of spiking (roughly 5 μg/kg). The outcome proves that the procedure used to prepare liquid milk spiked with chemical elements is suitable to produce in-house reference materials stable enough for analytical purposes. Furthermore, this procedure is easy to perform and can be applied by routine laboratories to produce samples for their IQC.

As proficiency tests (PTs) provider, the European Union Reference Laboratory for Chemical Elements in Food of Animal Origin (EURL-CEFAO) yearly organizes exercises on the determination of chemical elements within the area of its mandate. The scheme is addressed to the National Reference Laboratories (NRLs) of the European Union Member States. Each PT is planned giving priority to the matrices and elements for which maximum levels are set in Commission Regulation No. 1881/2006 and following amendments as well as to those mainly considered in National Residues Control Plans. Samples to be distributed are prepared in the Laboratory’s facilities using materials purchased on the market and often adjusting the concentration levels of the analytes around their maximum levels. In the 2006–2011 period, PTs were planned as a long-term programme pursuing the general objective of providing the NRLs with a scheme that can give them the opportunity to check and improve the performance of their analytical methods and to verify the effectiveness of any corrective actions through the repetition of the same matrix. Control charts give participants the possibility of a long-term follow-up of their performance promoting the improvement of Quality Control. To this aim, Shewhart and Cusum control charts for z-scores are prepared according to ISO 13528:2005 and updated after each PT for each laboratory. z-scores are assigned using values of σ pEURL-CEFAO that correspond to the level of performance appropriate to the demand. Cusum charts are also evaluated by EURL-CEFAO in order to identify problems that may cause a bias in the measurement method.

One of the emerging issues regarding the analysis of inorganic contaminants in food is the determination of Cadmium (Cd) and Lead (Pb) in honey. In fact, this kind of analysis is foreseen in most of the National Residue Control Plans (NRCPs) that European Union Member States (EU MSs) have to perform according to Directive 96/23.With the aim to provide technical support to the EU National Reference Laboratories (NRLs), an easy-to-use method on direct determination (DD) of Cd and Pb in honey by graphite furnace atomic absorption spectrometry (GF-AAS) after dissolution in an aqueous mixture of 2.5 % HNO3 (v/v) and 12.5 % H2O2 (v/v) was in-house validated and distributed to the NRLs network. Analyses were carried out on a batch prepared for the feasibility study of the EURL-CEFAO 19th PT on honey. The validation levels (20 and 100 µg/kg for Cd and Pb, respectively) were chosen similar to those that would have been proposed for the PT.The method proved its efficacy in terms of analytical performance; it appears to be low cost and time saving compared to a microwave sample preparation. In addition, it also decreases the environmental impact, being the amount of acid and reagents considerably reduced.

The ring-closing metathesis (RCM) reactions of homoallylic acrylates bearing alkyl substituents on various positions of their skeleton afford the corresponding pentenolides in the presence of carbene ruthenium catalysts. For R-3 = R-4 = H, or R-3 = Me, R-4 = H, the reactions are catalyzed by complex [RuCl2(PCy3)(2)(CHPh)], while a second-generation Grubbs catalyst is required when R-3 = H and R-4 = Me, R-3 = R-4 = Me, or R-3 = i-Pr and R-4 = H. Alkyl substitution at the homoallylic carbon (R-1, R-2) increases the yield of the reaction when both the acrylic and/or homoallylic double bonds are methyl-substituted. The interaction of the catalyst with the substrate in the initiation stage involves the homoallylic double bond rather than the acrylic moiety, and the resulting alkylidene species from the first-generation Grubbs catalyst can be observed by H-1 and P-31 NMR. The racemic tobacco constituents 4-isopropyl-5,6-dihydropyran-2-one and 4-isopropyltetrahydropyran-2-one are prepared via a short reaction sequence, involving the RCM reaction as the key transformation.

A proficiency test on the quantification of Al, Cu, Mn, Se and Zn in serum was carried out to verify the performance of about 30 regional laboratories of the network of Italian laboratories. The exercise consisted of four runs in which the laboratories were free in choosing analytical methods to determine trace elements in freeze-dried animal serum. Laboratories performances were evaluated by the study of statistical functions as Coefficients of Variation (CV), Youden plot and Z-score value. As for Al, the results were generally characterized by good accuracy and precision, in spite of the low levels of the element (5-7 microg l(-1)). Copper determination had some problems only at low concentration (about 160 microg l(-1)--first run), in which an elevated number of anomalous data were found. Better data were achieved for Zn, for which anomalous values were mainly stragglers than outliers. Due to the low number of data for Mn (concentrations from 0.6 to 60 microg l(-1)) and Se (concentration from 45 to 106 microg l(-1)), a restricted statistical treatment was applied; for these elements high CV values were found (range from 30 to 80%). The results of this trial confirmed that participation in a proficiency test represents a benefit for all analytical laboratories. In fact, with few exceptions, most of the participants improved their performances in terms of Z-score values.