High resolution NMR technique has been used to monitor post-mortem changes in salmon (Salmo salar) fillets upon storage at 4 and 0°C. Thirty-one different fish metabolites influencing freshness and taste properties have been unequivocally assigned by NMR using either available standard compounds or ad hoc acquired 2D (1)H-(1)H TOCSY and (1)H-(13)С HSQC spectra. The monitored fish metabolites include amino acids, dipeptides, sugars, vitamins, biogenic amines, as well as different products of the ATP degradation. The detection and monitoring of biogenic amines by NMR, upon fish storage, is information of interest for consumers, since some of these compounds are toxic. The data from this study shows that NMR spectroscopy also provides the amount of all metabolites necessary for the calculation of the K-index used to express fish freshness. A good correlation was found between the K-index increase and the formation of the undesired biogenic amines. The metabolite concentrations and the K-index found in this work were compared and found coherent with literature data. The performed study reveals the strengths and the suitability of the NMR approach to monitor different biochemical processes occurring during fish storage and qualitatively and quantitatively characterise fish metabolites determining fish quality.
The present work describes a foodomics protocol coupling an in vitro static simulation of digestion to a combination of omics techniques, to grant an overview of the protein digestibility of a meat-based food, namely Bresaola. The proteolytic activity mediated by the digestive enzymes is evaluated through Bradford and SDS-PAGE assays, combined to NMR relaxometry and spectroscopy, to obtain information ranging from the microscopic to the molecular level, respectively. The simple proteomics tool adopted here points out that a clear increase of bioaccessible proteins occurs in the gastric phase, rapidly disappearing during the following duodenal digestion. However, SDS-PAGE and the Bradford assay cannot follow the fate of the digested proteins when the products are sized <5 kDa. Conversely, NMR spectroscopy is able to capture the overall molecular profile of small fragments and peptides, which are mainly formed during the duodenal phase, thus giving the kinetics of the whole digestion process. Time domain NMR relaxometry, finally, detects the swelling phenomenon occurring during the gastric phase, when the digestion fluid enters the meat matrix.
The chemical composition of coffee has been widely investigated, focusing the attention both on main components and trace compounds. Most of these studies have been performed by using liquid and gas chromatography, eventually combined with mass spectroscometry. These techniques, although straight and effective, are time demanding due to the sample pretreatments. Here, we propose high‐resolution‐magic‐angle spinning nuclear magnetic resonance spectroscopy (HR‐MAS NMR), a system capable of acquiring highly resolved NMR spectra of gel‐like and suspension samples. This approach allowed us to determine the chemical composition of coarsely ground coffee beans of two varieties: Arabica and Robusta. Variation of the concentration of relevant species was monitored as a function of roasting temperature, from green beans to completely roasted. The HR‐MAS NMR tool demonstrated to be very powerful for quick chemical composition determination, opening up possibilities for novel applications of this approach in food quality control. PRACTICAL APPLICATIONS Food quality control needs novel and press‐button applications. High‐resolution‐magic‐angle spinning nuclear magnetic resonance contains such requirements, since it can analyze suspension and gel‐like samples, providing a chemical characterization with minor, or, in most cases, no chemical and physical pretreatment operations. The application proposed here concerns the examination of relevant molecules in coffee beans as a function of the roasting temperature. This can be used for a quality check of the final product, and such approach has a general suitability, being functional for almost all foodstuff, fresh and transformed.
Nuclear magnetic resonance spectroscopy was employed to obtain information about the changes occurring in Bogue ( Boops boops ) fish during storage. For this purpose, 1 H-NMR spectra were recorded at 600 MHz on trichloroacetic acid extracts of fish flesh stored over a 15 days period both at 4 °C and on ice. Such spectra allowed the identification and quantification of amino acids, together with the main organic acids and alcohols. The concentration of acidic and basic free amino acids was generally found to increase and decrease during storage, respectively. These concentration changes were slow during the first days, as a consequence of protein autolysis, and at higher rates afterward, resulting from microbial development. Two of the amino acids that showed the greatest concentration change were alanine and glycine, known to have a key role in determining the individual taste of different fish species. The concentration of serine decreased during storage, as highlighted in the literature for frozen fish samples. Differences in the amino acids concentration trends were found to be related to the different storage temperatures from day 4 onwards.
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