Giovanna Loredana La Torre

High performance liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry for sensitive determination of bioactive amines in donkey milk

In the present study we report on the optimization and validation of a sensitive high performance liquid chromatography atmospheric pressure chemical ionization mass spectrometry (HPLC-APCI-MS) method for the determination of 8 bioactive amines (histamine, tyramine, tryptamine, 2-phenylethylamine, cadaverine, putrescine, spermidine and spermine) in donkey milk samples. The method involves donkey milk pre-treatment to remove proteins and pre-column dansylation of the amines. HPLC in reversed phase mode has been used for bioactive amines separation and the operating condition of the APCI-MS system proved to be powerful and very efficient for peak assignment. The separation was accomplished in a short time with an excellent resolution for all the amine peaks. Quantification was carried out by monitoring the characteristic [M+H](+) ion of each amine derivative. The method sensitivity, linearity and repeatability were assayed with satisfactory results. The detection limits of the analysed amines ranged from 0.5 microg L(-1) to 15 microg L(-1); the highest LOD was for spermine. Also remarkably good recovery values were obtained; at the lowest spiking level (1 microg L(-1)) the percent mean recoveries ranged from 77.7 to 109.7. Furthermore, as the investigations relate to a complex matrix as donkey milk, suitable studies on matrix effect were performed. Finally, the developed and validated method was applied to analyse 13 donkey milk samples. Among the identified bioactive amines, putrescine, spermine and spermidine proved to be the main amines in donkey milk. Their concentration levels in the present study were lower than the values determined in mature human, cow and sow milk.

Determination of 1,2/1,3-diglycerides in Sicilian extra-virgin olive oils by (1)H-NMR over a one-year storage period.

Abstract This study is aimed to monitor by 1H NMR spectroscopy the effect of a 12-month storage period on the 1,2-diglycerides over 1,3-diglycerides ratio for five mono-cultivar ‘extra virgin olive oils’ (EVOO) (Arbequina, Arbosana, Cerasuola, Nocellara and FS17) and one blend of two different cultivars (Nocellara + Biancolilla) preserved in the dark and at room temperature. These quantifications, at 500 MHz, are readily extracted through a specific and original integration difference method. Albeit it was known that the isomerisation rate is affected by the free acidity, we here demonstrate that it also depends on the presence of specific macromolecules (lipases), indeed, different EVOO cultivars with similar free acidity, show different isomerisation rate. Our results are consistent with similar diglyceride monitoring performed on Greek and Spanish EVOOs by 31P NMR.

Interdonato lemon from Nizza di Sicilia (Italy): chemical composition of hexane extract of lemon peel and histochemical investigation

Abstract Considering that the determination of authenticity and of the geographical origin of food is a very challenging issue, in this study we studied by means of histological and histochemical analyses the famous Sicilian lemon known as ‘Interdonato Lemon of Messina PGI’. Since the protected geographical indication Interdonato lemon of Messina possesses high organoleptic properties, the composition of the hexane extract of lemon peel was determined by HRGC and HRGC–MS analyses and compared with that of lemon of different cultivars. The results obtained are informative of the oil’s quality and explain the variation of the lemon essential oil composition. Given the fundamental economic implications of any fraud, the aim of this study was to determine a fingerprint able to evaluate the authentication of the geographic origin in such way to prevent frauds in national and international markets. Graphical Abstract

The complexation of halide ions by acalix[6]pyrrole

The X-ray crystal structures of the 1∶1 complexes formed by calix[6]pyrrole 1b with Bun4NCl and Bun4NBr show the macrocycle to adopt D3d symmetry and to encapsulate the halide ions within the macroring cavity via six N–H···X– hydrogen bonds; the macrocycle subtly adjusts its conformation to accommodate the differently sized anions; preliminary extraction experiments indicate that 1b is a dramatically stronger chloride ion complexing agent than its smaller analogue calix[4]pyrrole 1a.

Fast UPLC/PDA determination of squalene in Sicilian P.D.O. pistachio from Bronte: optimization of oil extraction method and analytical characterization

A fast reversed-phase UPLC method was developed for squalene determination in Sicilian pistachio samples that entry in the European register of the products with P.D.O. In the present study the SPE procedure was optimized for the squalene extraction prior to the UPLC/PDA analysis. The precision of the full analytical procedure was satisfactory and the mean recoveries were 92.8±0.3% and 96.6±0.1% for 25 and 50mgL-1 level of addition, respectively. Selected chromatographic conditions allowed a very fast squalene determination; in fact it was well separated in ∼0.54min with good resolution. Squalene was detected in all the pistachio samples analyzed and the levels ranged from 55.45-226.34mgkg-1. Comparing our results with those of other studies it emerges that squalene contents in P.D.O. Sicilian pistachio samples, generally, were higher than those measured for other samples of different geographic origins.

Chemical Modifications of Furan-Based Calixarenes by Diels–Alder Reactions

The Diels–Alder reactions of the cyclic hexamer of furan and acetone C 6 with benzyne and DMAD (dimethylacetylenedicarboxylate) are described. In this way, C 6 can be exploited as a framework on which to place sets of carboxyl functions to obtain a novel family of furan-based calixarenes, such as 1, with potential applications in supramolecular chemistry.

Toxic inorganic pollutants in foods from agricultural producing areas of Southern Italy: Level and risk assessment

This study focused on the inorganic environmental contaminants in specific food products which form part of the food chain of the population residing in the area of Southern Italy (Gela) where there is a high mortality rate linked to tumor diseases and congenital malformations. Determination of toxic metals was performed by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). The toxicological data for every toxic element has been applied to evaluate the risk for the consumer by calculating the amount of potentially toxic element that would ingest an average of 60kg weight individual adult. The analysis of the investigated samples shows a high level of metal contamination which can be linked both to the polluted water and air. The obtained results give us an idea about the agricultural products contamination and possible exposure of local people through the food chain.

Determination and quantification of PCBs, POCs and PAHs in Thunnus thynnus from the Straits of Messina (Italy)

This data set is composed to assess the accumulation of persistent organic pollutants (POPs) such as polychlorinated biphenyls (PCBs) dioxin like (DL) and not dioxin like (NDL), organochlorine pesticides (POCs) and polycyclic aromatic hydrocarbons (PAHs) in Thunnus thynnus and to elucidate the suitability of this species as a bioindicator for monitoring contaminations of these compounds in the marine ecosystems of the Straits of Messina. This investigation was conducted on liver samples of 14 T. thynnus collected during April 2015. Quantitative determination of PCBs (DL and NDL), POCs and PAHs in the examined samples has been carried out by HRGC-MS/MS. Among the PCBs, high prevalence of DL was found while, generally, the values detected for PCBs–NDL were lower than the legal limits. Tuna samples analyzed for PAHs residues revealed that all the samples were contaminated with acenaphthalene, fluorene, phenanthrene and anthracene. Moreover, generally the residual levels of DDT and DDT metabolites were low. The total content of PCB–DL, in almost all the samples, showed higher concentration than the legal limit.

Compounds with Antioxidant Properties in Pistachio (Pistacia vera L.) Seeds

Publisher Summary This chapter outlines the antioxidants found in pistachio seeds and their benefits to human health. Different antioxidant classes are present in pistachio seeds: anthocyanins, tocopherols, carotenoids, chlorophylls, flavonoids, isoflavones, proanthocyanidins, anacardic acids, and cardanols, as well as resveratrol and vitamin C. These antioxidants can interact in very different ways: the synergistic effects can improve the protection against oxidative damage and play an important role in the biological antioxidant network. Hydrophilic extracts of pistachio nuts inhibited both the metal-dependent and the metal-independent lipid oxidation of bovine liver microsomes and also the Cu2+-induced oxidation of human low density lipoproteins. Studies of the benefits of pistachio consumption in humans show that the mean plasma total cholesterol and malondialdehyde levels, total cholesterol/high density lipoprotein ratio, and low density lipoprotein/high density lipoprotein ratio significantly decrease. The use of antioxidants as chemopreventive agents by inhibiting radical generation has been suggested, since free radicals are responsible for DNA damage and scavengers are probably important in cancer prevention.

Development of minimal fermentation media supplementation for ethanol production using two Saccharomyces cerevisiae strains

Abstract Ethanol production by fermentation is strongly dependent on media composition. Specific nutrients, such as trace elements, vitamins and nitrogen will affect the physiological state and, consequently, the fermentation performance of the micro-organism employed. The purpose of this study has been to assess the highest ethanol production by a minimal medium, instead of the more complex nutrients supplementation used during alcoholic fermentation. All fermentation tests were carried out using a microwell plate reader to monitor the processes. Two Saccharomyces cerevisiae strains (NCYC 2826 and NCYC 3445) were tested using three nitrogen sources, supplied with different vitamin and salts. The results show that solutions made of urea phosphate, KCl, MgSO4·7H2O, Ca-panthothenate, biotin allowed an ethanol yield of 22.9 and 23.4 g/L for strain NCYC 2826 and NCYC 3445, respectively, representing 90 and 92% of the theoretical yield. All tests were carried out using glucose as common reference carbon source.