72 research outputs found
catena-Poly[bis(4-aminopyridinium) [[tetraaquanickel(II)]-μ-benzene-1,2,4,5-tetracarboxylato] dihydrate]
The asymmetric unit of the title compound, {(C5H7N2)2[Ni(C10H2O8)(H2O)4]·2H2O}n, contains an NiII atom, two water molecules of coordination, one half of a benzene-1,2,4,5-tetracarboxylate (btec) anionic ligand, one 4-aminopyridinium cation (papy) and an uncoordinated water molecule. The metal center lies on an inversion center and adopts an octahedral geometry with the carboxylate groups tilted out of the mean plane formed by the btec. In the crystal, molecules are linked into one-dimensional coordination polymers running along the ac diagonal. The crystal structure is consolidated by N—H⋯O and O—H⋯O hydrogen bonds
Determination and quantification of carotenoids in sea sponges Raspaciona aculeata and Dictyonella marsilii present in the Ganzirri Lake (Messina), Italy
Considering the crucial role of carotenoids exploitable both as nutraceuticals and also as dyes in food industry, there are many efforts in seeking for new sources of these pigments, especially in the marine world. In this study, for the first time, we extracted carotenoids from sea sponges Raspaciona aculeata and Dictyonella marsilii taken from Ganzirri Lake Messina (Italy). The determination and quantification of carotenoids was made by UPLC-PDA-MS. Remarkable results concern renieratene content in R. aculeate found to be over 2570 ppm
Expanding the knowledge related to flavors and fragrances by means of three-dimensional preparative Gas Chromatography and Molecular Spectroscopy
As universally known, gas chromatography (GC) coupled with mass spectrometry (MS) allows us to acquire spectra that can be searched in specific databases to attain qualitative information on a peak of interest. When not present in databases, structure elucidation is required before including a new component in a library: from that moment, scientists all around the world will be able to identify the new molecule with analytical confidence after GC-MS analysis. Conversely, if data are not shared in commercial databases, even if a molecule is studied and elucidated, it appears to be unknown or only identifiable on the basis of third-party data taken from the literature, which is a serious limitation. The present paper deals with a case that confirms this assumption. A component of Myrtus communis L. volatile fraction was tentatively identified based on literature data. Despite this, reliable identification could not be achieved due to the lack of a corresponding spectrum in commercial MS databases. Afterwards, the target component was isolated in a reasonable quantity and with a high degree of purity for downstream characterization by spectroscopic techniques. For this purpose, preparative (prep) GC may appear insufficient for the isolation of volatile components from highly complex samples. In this study, a prep-MDGC system was implemented for the isolation of the compound of interest from myrtle oil, consisting of three wide-bore columns of different selectivity coupled by means of Deans switch transfer devices. Based on the NMR and GC-FTIR data acquired, the unknown compound was identified as 2,2,5,5,7,7-hexamethyl-3,7-dihydro-1-benzofuran-4,6(2H,5H)-dione. Noticeably, this is a known molecule, yet its mass spectrum had never been registered into MS databases and thus was not available to the scientific community. Finally, the spectrum was included for the first time in a commercial library, namely the FFNSC 5.0 MS database. The aim of the present study was to highlight the opportunity to make analytical data quickly available in a reliable way by registering them in searchable MS databases to improve the identification means for researchers all over the worl
catena-Poly[[[μ-aqua-pentaaquadizinc(II)]-μ4-benzene-1,2,4,5-tetracarboxylato] dihydrate]
The asymmetric unit of the title compound, {[Zn2(C10H2O8)(H2O)6]·2H2O}n, contains two distinct Zn atoms joined by a bridging water molecule and two bridging carboxylate groups belonging to distinct halves of benzene-1,2,4,5-tetracarboxylate (tbec) tetraanionic ligands, both lying on crystallographic inversion centres. The structure of this new isopolymorphic one-dimensional coordination polymer features asymmetric bimetallic octahedral knots. O—H⋯O hydrogen bonds between water molecules and carboxylate O atoms help to consolidate the crystal packing
Properties of a new food supplement containing actinia equina extract
Marine species represent a great source of biologically active substances; Actinia equina (AE),
an Anthozoa Cnidaria belonging to the Actinidiae family, have been proposed as original food and have
already been included in several cooking recipes in local Mediterranean shores, and endowed with
excellent nutraceutical potential. The aim of this study was to investigate some unexplored features
of AE, through analytical screening and an in-vitro and in-vivo model. An in-vitro study, made on
RAW 264.7 stimulated with H2O2, showed that the pre-treatment with AE exerted an antioxidant
action, reducing lipid peroxidation and up-regulating antioxidant enzymes. On the other hand,
the in-vivo study over murine model demonstrated that the administration of AE extracts is able
to reduce the carrageenan (CAR)-induced paw edema. Furthermore, the histological damage due
to the neutrophil infiltration is prevented, and this highlights precious anti-inflammatory features
of the interesting food-stu. Moreover, it was assessed that AE extract modulated nuclear factor
kappa-light-chain-enhancer of activated B cells (NF-kB) and The nuclear factor erythroid 2–related
factor 2 (Nrf-2) pathways. In conclusion, our data demonstrated that thanks to the antioxidant and
anti-inflammatory properties, AE extract could be used as a new food supplement for inflammatory
pathology prevention
A Fast and Efficient Ultrasound-Assisted Extraction of Tocopherols in Cow Milk Followed by HPLC Determination
A fast HPLC method with fluorescence detector (FD) was developed for the determination of three tocopherols (TOCs) in milk samples from Modicana cattle breed. The ultrasound-assisted procedure was optimized for the extraction of TOCs prior to HPLC/FD analysis, reducing sample preparation time and allowing a fast quantification of α-tocopherol, δ-tocopherol and γ tocopherol. The optimized ultrasonic extraction combines an efficient and simple saponification at room temperature and a rapid HPLC quantification of TOCs in milk. The precision of the full analytical procedure was satisfactory and the recoveries at three spiked levels were between 95.3% and 87.8%. The linear correlations were evaluated (R2 > 0.99) and the relative standard deviation (RSD) values for intra-day and inter-day tests at three spiked levels were below 1% for the retention time and below 5.20% for the area at low level spiking. The proposed procedure, reducing the experimental complexity, allowed accurate extraction and detection of three TOCs in milk samples from Modicana cattle breed
Targeted chemical characterization of the Pistacia Vera fruits by an innovative NMR approach
These data are the supplementary electronic material of the paper "Targeted chemical characterization of the Pistacia Vera fruits by an innovative NMR approach" submitted to the journal "Food Analytical Methods
PROTOCOLLO NMR E TRATTAMENTO DATI VERSO UNA RAPIDA E COMPLETA ETICHETTA NUTRIZIONALE PER OLII DI OLIVA
La grande potenzialità della risonanza magnetica nucleare nell’analisi degli olii di
oliva è ben nota [1] e dipende: a) dall’assenza di veri trattamenti chimici, b) dalla
costanza della risposta strumentale (buona riproducibilità), c) dalla rapida acquisizione
di molti dati, d) la quantificazione viene basata su una risposta chimico-fisica
dipendente solo dal momento magnetico nucleare che teoricamente rende le misure
quantitative valide in senso assoluto.[2] Per il rilevamento di composti minori, i noti
problemi di sensibilità imposti dal divario di rilevazione dinamico sono molto ridotti
grazie a tecniche di selezione spettrale [3] o pre-saturazione multipla [4]. La gran parte
degli studi NMR sfrutta le analisi statistiche multi-variate come mezzo di distinzione
tra classi omologhe (cultivar, locazione) di olii; d’altra parte, da un punto di vista
meramente scientifico, ogni olio è una miscela complessa di composti chimici di cui
conoscere la natura e la quantità. Quest’ultimo punto ha focalizzato i nostri sforzi
verso lo sviluppo di un protocollo combinato di tre esperimenti che possa fornire, in
tempi relativamente rapidi, la miglior etichetta nutrizionale possibile per un olio
ovviamente con le migliori possibili deviazioni standard. Gli esperimenti sono
fondamentalmente: a) lo spettro protonico 1H-NMR; b) lo spettro selettivo 1H-NMR
della zona aldeidica 8-10 ppm; c) Spettro del 13C-NMR. Questi spettri si rivelano
complementari in quanto lo spettro protonico è il più sensibile per i componenti
principali (esteri grassi, trigliceridi, di gliceridi e squalene) pur presentando molte
sovrapposizioni di segnali, lo spettro selettivo DPFGSE (Fig. 1) consente la
rilevazione degli importanti composti minori (polifenoli della famiglia dei
secoiridoidi), lo spettro di 13C, pur essendo meno sensibile, risulta molto selettivo
riducendo le sovrapposizioni. La combinazione ed elaborazione della gran mole di dati
ricostruisce in maniera coerente la composizione chimica dei campioni che tiene sotto
controllo anche le aberrazioni sperimentali grazie al concetto che ogni composto si
palesa tramite numerose evidenze strumentali (tutte le risonanze protoniche e tutte le
risonanze al 13C) a differenza di quanto accade nelle altre tecniche analitiche
NMR Detection of specific minor components separated by complex matrices such as extra-virgin olive oil (EVOO)
Comprehensive Chemical Characterization of the Pistacia vera Fruits through Original NMR Quantification Methods
(1) Background: Pistacia vera is a dry fruit spread all over the world, commonly known as pistachio, and is very appreciated as a snack, as a precious ingredient for confectionery industries and also as a blessed touch for gourmet dishes; (2) Methods: The simultaneous NMR profiles concerning the hydrophilic and hydrophobic phases, enabled by a specific throughput over grinded pistachio seeds, led to the comprehensive chemical characterization of these nuts coming from different territories; (3) Results: The customized extraction method is described in detail as well as the employed nuclear magnetic resonance (NMR) experiments. The chemical quantification takes advantage from the innovative multi-assignment recovered analysis (MARA-NMR) technique able to provide experimentally robust panels for both hydrophobic and hydrophilic chemicals. Beyond the assessed repeatability and the interesting statistical discrimination, this paper adds information about the quantitative and qualitative composition of pistachio as inferred by NMR data. This updated background can pave the way toward the development of wider and wider chemical panels improving the knowledge about the pistachio’s composition. This approach can be easily extended to other matrices
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