Search Results (103)

In food processing, non-destructive and non-invasive characterization is a powerful tool for monitoring processes and controlling quality. Cheeses consist of a large variety of products whose nutritional and sensory properties depend on the source materials, cheesemaking procedures, and biochemical transformations occurring during maturation and storage. In this study, proton magnetic resonance relaxation time correlation maps (2D ¹H-NMR T₁–T₂) are used to investigate the effect of the ripening degree on Pecorino cheese and evaluate its evolution during storage in a refrigerator under vacuum-packaging conditions. NMR relaxometry has allowed for non-invasive monitoring of packaged Pecorino cheese slices, and the results were compared with those obtained with the two widely used techniques, i.e., Differential Scanning Calorimetry (DSC) and Attenuated Total Reflectance Fourier-Transform Infrared Spectroscopy (ATR-FTIR). The analysis of variance and simultaneous component analysis (ASCA), separately applied to 2D ¹H-NMR T₁–T₂ correlation maps, DSC, and ATR-FTIR data, suggests that the results obtained with the NMR approach are consistent with those obtained using the two benchmark techniques. In addition, it can distinguish cheeses stored for different durations (storage time) irrespective of their original moisture content (ripening degree), and vice versa, without opening the vacuum-package, which could compromise the integrity of the samples. Full article

Nuclear Magnetic Resonance (NMR) and Magnetic Resonance Imaging (MRI) are powerful techniques that have been employed to analyze foodstuffs comprehensively. These techniques offer in-depth information about the chemical composition, structure, and spatial distribution of components in a variety of food products. Quantitative NMR is widely applied for precise quantification of metabolites, authentication of food products, and monitoring of food quality. Low-field ¹H-NMR relaxometry is an important technique for investigating the most abundant components of intact foodstuffs based on relaxation times and amplitude of the NMR signals. In particular, information on water compartments, diffusion, and movement can be obtained by detecting proton signals because of H₂O in foodstuffs. Saffron adulterations with calendula, safflower, turmeric, sandalwood, and tartrazine have been analyzed using benchtop NMR, an alternative to the high-field NMR approach. The fraudulent addition of Robusta to Arabica coffee was investigated by ¹H-NMR Spectroscopy and the marker of Robusta coffee can be detected in the ¹H-NMR spectrum. MRI images can be a reliable tool for appreciating morphological differences in vegetables and fruits. In kiwifruit, the effects of water loss and the states of water were investigated using MRI. It provides informative images regarding the spin density distribution of water molecules and the relationship between water and cellular tissues. ¹H-NMR spectra of aqueous extract of kiwifruits affected by elephantiasis show a higher number of small oligosaccharides than healthy fruits do. One of the frauds that has been detected in the olive oil sector reflects the addition of hazelnut oils to olive oils. However, using the NMR methodology, it is possible to distinguish the two types of oils, since, in hazelnut oils, linolenic fatty chains and squalene are absent, which is also indicated by the ¹H-NMR spectrum. NMR has been applied to detect milk adulterations, such as bovine milk being spiked with known levels of whey, urea, synthetic urine, and synthetic milk. In particular, T2 relaxation time has been found to be significantly affected by adulteration as it increases with adulterant percentage. The ¹H spectrum of honey samples from two botanical species shows the presence of signals due to the specific markers of two botanical species. NMR generates large datasets due to the complexity of food matrices and, to deal with this, chemometrics (multivariate analysis) can be applied to monitor the changes in the constituents of foodstuffs, assess the self-life, and determine the effects of storage conditions. Multivariate analysis could help in managing and interpreting complex NMR data by reducing dimensionality and identifying patterns. NMR spectroscopy followed by multivariate analysis can be channelized for evaluating the nutritional profile of food products by quantifying vitamins, sugars, fatty acids, amino acids, and other nutrients. In this review, we summarize the importance of NMR spectroscopy in chemical profiling and quality assessment of food products employing magnetic resonance technologies and multivariate statistical analysis. Full article

Determining the technological quality of fresh meat pieces is essential in the meat industry to ensure the production of high-quality products. For this purpose, nuclear magnetic resonance (NMR) is a non-destructive and non-invasive technique that appears as an alternative to traditional methodologies. The objective of this work is to determine the potential of magnetic resonance imaging (MRI) and time-domain (TD-NMR) relaxometry for determining the physicochemical characterization of fresh hams with different industrial destinations (both fresh and cured products, such as dry-cured ham). For this study, the biceps femoris, semimembranosus, and semitendinosus muscles of 20 fresh hind legs from white pigs, classified into four categories according to their fat content, were analyzed. The semitendinosus muscle was selected as a model, and positive and negative correlations were obtained between different physicochemical parameters and the longitudinal (T1) and transverse (T2) relaxation times obtained by MRI and TD-NMR. Regression models using T1 and T2 were also developed to predict the muscle water-holding capacity (WHC) and drip loss, using high, medium, and low magnetic field NMR (R² > 0.80). Therefore, MRI and TD-NMR could be considered as highly suitable and accurate non-destructive techniques for the WHC determination in the meat industry. Full article

Concrete printing technologies play a key role in the modernization of construction practices. One factor that mitigates their progress is the development of standards and characterization tools for concrete during printing. The aim of this work is to point out correlations between some printability descriptors of mortars and the data obtained from low-field nuclear magnetic resonance (NMR) relaxometry techniques. In this context, the superposed effects of an acrylic-based superplasticizer and calcium nitrate accelerator were investigated. The mortars under study are based on white Portland cement, fine aggregates, and silica fume at fixed ratios. Extrusion tests and visual inspection of the filaments evaluate the extrudability and the printing window. The selected compositions were also investigated via transverse $\left(T_2\right)$ and longitudinal $\left(T_1\right)$ NMR relaxation times. The results indicate that both additives increase the printing window of the mortar, while the accelerator induces a faster increase in specific surface area of capillary pores $\left(S/V\right)$ only after 30–60 min of hydration. Some correlations were found between the printing window and the range where the transverse relaxation rates $\left(1/T_2\right)$ and the pore surface-to-volume ratios $\left(S/V\right)$ increase linearly. This suggests some promising connections between NMR techniques and the study of structural buildup of cementitious materials. Full article

The increasing demand for diverse foods and tailored nutrition encourages the development of innovative products, such as bread enriched with cricket powder (CP) or potato protein (PP). This study presents the preparation and analysis of gluten-free breads with CP and PP, focusing on their nutritional value and physical properties. Analytical methods included water activity measurement, bread volume, crumb color analysis, FTIR spectroscopy, low-field NMR relaxometry, and texture profile analysis. Ash content ranged from 0.60 ± 0.03% to 1.16 ± 0.11%, and caloric values ranged from 216.2 to 229.5 kcal/100 g. Water activity remained stable across all samples (0.975–0.976). Crumb color analysis showed the greatest change in CP samples (ΔE = 14.07), while PP had minimal impact (ΔE = 2.15). FTIR spectra revealed increased amide I and II bands, indicating higher protein content. NMR results demonstrated shorter T₁, T₂₁, and T₂₂ times for CP, suggesting reduced water mobility and a denser structure, while PP samples showed higher values, indicating a looser, more hydrated matrix. Texture analysis confirmed that CP increased firmness and compactness, whereas PP enhanced springiness. These findings suggest that CP and PP can improve the nutritional and structural properties of gluten-free bread, offering valuable alternatives for modern dietary needs. Full article

The physical stability, molecular mobility, and appearance of nanocrystalline resveratrol in a polyvinylpyrrolidone (PVP) matrix were investigated. Two formulations with resveratrol loadings of 30% and 50% were prepared and characterized using powder X-ray diffraction (PXRD) and time-domain nuclear magnetic resonance (TD-NMR). Samples were studied over time (up to 300 days post-preparation), across temperatures (80–300 K), and under varying humidity conditions (0% and 75% relative humidity). The results demonstrate that the 30% resveratrol–PVP sample is a homogeneous amorphous solid dispersion (ASD), while the 50% resveratrol–PVP sample contained resveratrol nanocrystals measuring about 40 nm. NMR measurements and molecular dynamics (MD) simulations revealed that incorporation of resveratrol into the polymer matrix modifies the system’s dynamics and mobility compared to the pure PVP polymer. Additionally, MD simulations analyzed the hydrogen bonding network within the system, providing insights for a better understanding of the physical stability of the ASD under different conditions. Full article

Background/Objectives: Colorectal cancer (CRC) is one of the most common and deadly types of cancer. Compared with the classical histopathological approach, this study discusses the application of ¹H NMR and FT-IR techniques for the fast evaluation degree of healing of patients with CRC after surgical intervention. Methods: Native and deproteinized blood plasma collected from 10 patients with confirmed CRC and 20 healthy volunteers were analyzed using ¹H NMR T₂ distributions and FT-IR spectra measured for samples collected before and 7 days after surgery. The average FT-IR spectrum from 20 healthy volunteers is also presented. Principal component analysis (PCA) was performed on the FT-IR spectra. The results were used for further statistical analysis using receiver operating characteristic (ROC) and area under the curve (AUC) and to produce a series of prediction maps using a machine learning library. Results: Both experimental methods combined with analysis methods demonstrated that the native blood plasma samples can be better used to predict the CRC patients’ evolution 7 days after surgery. Three patients showed a significant evolution by ¹H NMR T₂ distribution, correlated to the observation of FT-IR–PCA analysis. Maps of medical state probability were generated using a trained machine learning-based ANN. Conclusions: The experimental measurements combined with an advanced statistical analysis and machine learning were successfully used and show that the healing process of patients with CRC is not linear, from the preoperative state to the state associated with healthy volunteers, but passes through a distinct healing state Full article

This study investigates the functionalization of a poplar biochar (PB), obtained by high-temperature pyrolysis, under oxidative conditions typically used in organic synthesis. In particular, concentrated nitric acid, a sulfonitric mixture and a piranha mixture were applied as oxidants at different temperatures and reaction times. In order to assess the outcome of the reaction conditions on the characteristics of the resultant products, these were characterized by a combination of imaging (SEM), spectroscopic (ATR-FTIR, RAMAN) and FFC-NMR relaxometric techniques. The latter techniques, rationalized in terms of the Kohlrausch-type stretched exponential kinetic model, were analyzed using a recently developed heuristic Monte Carlo method, providing insights into the water dynamics within material pore networks. Additionally, the water-holding capacity of the modified biochars and their abilities to adsorb some model dyes were evaluated. The results clarify the relationship between oxidative treatment conditions and biochar properties, highlighting their impact on both structural modifications and water dynamics within the porous network, and enabling us to identify the best reaction conditions for optimizing the features of the oxidized product. Full article

In this study, we report the findings of a morphological analysis of a resorcinol–formaldehyde (RF)-based carbon aerogel (CA) and its graphene oxide (GO)-doped version (CA-GO), prepared for possible applications as an electrode material. Beyond some electron microscopic and N₂ sorption investigations, we mostly used NMR cryoporometry and relaxometry to characterize the gels in a wet state, as they are usually applied. The precursor RF polymer aerogel was prepared both with and without GO and was subsequently carbonized into carbon aerogel. Modifying the polymer aerogel using GO resulted in a larger variety of C-O bonds in both polymer aerogels. However, the most important changes occurred in the morphology of the carbon aerogels. NMR relaxometry revealed the highly hydrophilic nature of the pore wall of the RF polymer aerogels, as demonstrated by their uniform wetting behavior. The carbonization resulted in a mostly hydrophobic pore wall decorated by some oxygen-containing spots and a macroporous system. Doping with GO after pyrolysis resulted in spherical pores in the CA and cylindrical pores in the CA-GO, which is potentially a more promising material for electrochemical use than CA. Full article

This study presents a fast, non-invasive method to determine the iodine value (IV) of edible oils using Time Domain Nuclear Magnetic Resonance (TD-NMR) and Magnetic Resonance Imaging (MRI) techniques. The IV, which quantifies the degree of unsaturation in fats and oils, is a key parameter in assessing oil quality and detecting potential adulteration. Different edible oils were used in this study (sunflower, soy, olive, sesame, and linseed). Statistically significant regression models (R² > 0.92) were established between the IV derived from NMR spectra and the longitudinal (T1) and transverse (T2) relaxation times of the oils, which were obtained from MRI and TD-NMR analyses. The regression models obtained allow for the prediction of the IV from the T1 and T2 relaxation times across a range that includes predominantly mono- and polyunsaturated edible vegetable oils. The TD-NMR approach stands out for its speed (<2 min), lack of sample preparation (including direct analysis within the commercial packaging), and reproducibility, with a variability of only 0.62%. Meanwhile, the MRI technique allows for the simultaneous evaluation of multiple samples in a single acquisition. Together, these features make TD-NMR and MRI effective tools for the rapid and reliable analysis of the IV in edible oils. Full article

The purpose of this research is to design nanocomposite materials for biomedical applications. New conjugates of PEG derivatives of RGD peptides and magnetic nanoparticles, based on Fe₃O₄ (MNPs) with silica coating covalently labelled with fluorescent dye Cyanine5, were obtained. It was shown that a higher loading level of RGD peptides occurred in the case of MNPs with SiO₂/aminopropylsilane coating, synthesised using N-(phosphonomethyl)iminodiacetic acid (PMIDA) as a surfactant. To confirm the structure and chemical purity of the new RGD-PEG conjugate, a number of methods were used, including ¹H NMR, HRMS, and RP-HPLC. The characterisation of MNPs was carried out using the following physical methods: TEM, FTIR, EDX, CHN analysis, DLS, fluorescence spectrometry, vibration magnetometry, and relaxometry. Samples obtained from PMIDA-stabilised MNPs contained a greater amount of the peptide and possessed better hydrodynamic characteristics than samples obtained from non-stabilised MNPs. A comparative study of the MNP cytotoxicity was carried out towards 4T1 and MDA-MB231 cell lines (MTT test), and the possibility of cell labelling was assessed. The cellular uptake was more efficient for nanoconjugates obtained without PMIDA. The data obtained can be used for the design of materials for cell labelling and visualisation. Full article

Objectives: Hydrogels produced using the freeze–thaw method have demonstrated significant potential for wound management applications. However, their production requires precise control over critical factors including freezing temperature and the choice of matrix-forming excipients, for which no consensus on the optimal conditions currently exists. This study aimed to address this gap by evaluating the effects of the above-mentioned variables on cryogel performance. Methods: Mechanical properties, absorption capacity, and microstructure were assessed alongside advanced analyses using differential scanning calorimetry (DSC) and low-field nuclear magnetic resonance relaxometry (LF TD NMR). Results: The results demonstrated that fully hydrolyzed polyvinyl alcohol (PVA) with a molecular weight above 61,000 g/mol is essential for producing high-performance cryogels. Among the tested formulations, an 8% (w/w) PVA_56–98 solution (Mw~195,000; DH = 98.0–98.8%) with 10% (w/w) propylene glycol (PG) provided the best balance of stretchability, durability, and low adhesion. Notably, while −25 °C is often used for cryogel preparation, freezing the gel precursor at −80 °C yielded superior results, producing materials with more open, interconnected structures and enhanced mechanical strength and elasticity—deviating from conventional practices. Conclusions: The designed cryogel prototypes exhibited functional properties comparable to or even surpassing commercial wound dressings, except for absorption capacity, which remained lower. Despite this, the cryogel prototypes demonstrated potential as wound dressings, particularly for use in dry or minimally exuding wounds. All in all, this study provides a comprehensive analysis of the physicochemical and functional properties of PVA cryogels, establishing a strong foundation for the development of advanced wound dressing systems. Full article

Using liquid crystals in near-infrared applications suffers from effects related to processes like parasitic absorption and high sensitivity to UV-light exposure. One way of managing these disadvantages is to use deuterated systems. The combined ¹H and ²H nuclear magnetic resonance relaxometry method (FFC NMR), dielectric spectroscopy (DS), optical microscopy (POM), and differential scanning calorimetry (DSC) approach was applied to investigate the influence of selective deuteration on the molecular dynamics, thermal properties, self-organization, and electric-field responsiveness to a 4′-pentyl-4-biphenylcarbonitrile (5CB) liquid crystal. The NMR relaxation dispersion (NMRD) profiles were analyzed using theoretical models for the description of dynamics processes in different mesophases. Obtained optical textures of selectively deuterated 5CB showed the occurrence of the domain structure close to the I/N phase transition. The dielectric measurements showed a substantial difference in switching fields between fully protonated/deuterated 5CB and selectively deuterated molecules. The DSC thermograms showed a more complex phase transition sequence for partially deuterated 5CB with respect to fully protonated/deuterated molecules. Full article

Biosolids from stabilized sludge present a high fertilization potential, due to their rich content of nutrients and organic matter. The intrinsic and subtle properties of such fertilizers may greatly influence the fertilization efficiency. In this sense, the utility, advantages and limitations of advanced characterization methods, for the investigation of structural and dynamic properties at the microscopic scale of slightly different formulations of fertilizers were assessed. For that, three formulas of organo-mineral fertilizers based on biosolids (V1, V2 and V3), having at least 2% N, 2% P₂O₅, and 2% K₂O, were characterized by advanced methods, such as ¹H NMR relaxometry, ¹H MAS and ¹³C CP-MAS NMR spectroscopy, ¹H double-quantum NMR and FT-IR spectroscopy. Advanced structural characterization was performed using SEM, EDX and X-ray diffraction. Four dynamical components were identified in the NMR T₂ distribution showing that the rigid component has a percentage larger than 90%, which explains the broad band of NMR spectra confirmed by the distributions of many components in residual dipolar coupling as were revealed by ¹H DQ-NMR measurements. SEM and EDX measurements helped the identification of components from crystalline-like X-ray diffraction patterns. To evaluate the release properties of organo-mineral fertilizers, dynamic measurements of classical electric conductivity and pH were performed by placing 0.25 g of the formulas (V1, V2 and V3) in 200 mL of distilled water. The content of N and P were quantified using specific reactants, combined with VIS-nearIR spectroscopy. Two release mechanisms were observed and characterized. It was found that V3 presents the smallest release velocity but releases the largest number of fertilizers. Full article

Asphalt binder performance grades (PGs) are important metrics in designing pavements for effective transportation infrastructure. The PG system relies on the binder’s stiffness and is determined through energy- and time-intensive physical testing. Physical properties, like stiffness, can also be determined by spin–lattice NMR relaxometry, a non-destructive chemical method. NMR relaxometry can quantify the molecular mobility of materials by determining relaxation times from exponential decays of excited nuclear magnetization. While relaxation times have been used to determine physical properties of materials, a quantitative relation to the PG grades of asphalt binder is yet to be established. In this study, T₁ NMR relaxation analyses were used to differentiate between solid asphalt binders and determine the fastest yet still-reliable method of modeling exponential decay data. Algorithms that fit exponential decay relaxation data using one, two, or three independent relaxation times were compared with a 128-coefficient discrete inverse Laplace transformation to determine the best mathematical fit for a comparative analysis. The number of data points was then reduced from 256 to 64 to 16 and finally to 8 data points on a relaxation curve to reduce the testing time and determine the minimum number of data points needed for comparison. Two batches of PG 64-22 asphalt binder, along with samples of PG 76-22 and 94-10 binders, were investigated. The best compromise between measuring time and data reliability was found by acquiring 64 data points and then using a biexponential model to fit the experimental data. The PG 64-22 sources provided similar results, indicating similar physical properties. The PG 64-22 and PG 76-22 binders could also be compared via monoexponential data fits, but the PG 94-10 samples required an additional relaxation parameter for comparison. To differentiate all three binder grades, the primary relaxation times, along with their relative ratios, were utilized. Full article