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1.
Anal Chem ; 94(44): 15223-15230, 2022 11 08.
Article in English | MEDLINE | ID: mdl-36302263

ABSTRACT

Combining spectroscopic techniques with electrochemistry is a promising strategy, as it allows the detailed investigation of the species that are consumed and produced by the reaction in real time. However, as with any in situ coupling technique, the junction between NMR and electrochemistry presents some challenges, notably the distortion of NMR signals due to the placement of electrodes close to or within the detection region. In this work, miniaturized electrodes made of carbon fiber paper were developed and later modified with platinum. Platinum decoration by cathodic deposition was chosen, as platinum is a prominent element in electrocatalysis, able to catalyze a large variety of reactions. To evaluate the efficiency of this electrochemical system, the oxidation of ascorbic acid was used as a model reaction. It was observed that the electrodes caused substantial signal distortion when placed within the detection region (full width at half-maximum equal to 1.46 Hz), whereas no distortion was observed when the electrodes were placed 1 mm above the detection region (full width at half-maximum equal to 0.95 Hz). With this system, it was also possible to monitor the magnetoelectrolysis effect, caused by the interaction of the magnetic field with the flowing ions, leading to a doubling of the ascorbic acid oxidation rate, compared to the reaction performed without a magnetic field. In addition to its low cost and simplicity in preparation, the developed electrode system allows the electrode surface to be easily modified with other suitable catalysts.


Subject(s)
Ascorbic Acid , Platinum , Microelectrodes , Carbon Fiber , Platinum/chemistry , Electrodes , Electrochemistry , Oxidation-Reduction , Carbon/chemistry
2.
Carbohydr Polym ; 250: 116891, 2020 Dec 15.
Article in English | MEDLINE | ID: mdl-33049828

ABSTRACT

We propose a novel approach relied on high-resolution solid-state 13C NMR spectroscopy to quantify the crystallinity index of chitosans (Ch) prepared with variable average degrees of acetylation (DA¯) from 5% to 60 % and average weight molecular weight (M¯w) ranged in 0.15 × 106 g mol-1-1.2 × 106 g mol-1. The Dipolar Chemical Shift Correlation (DIPSHIFT) curve of the C(6)OH segment revealed increased mobility dynamic, which induced different distribution from trans-to-gauche conformations in relation to C(4). Indeed, 1H-13C Heteronuclear Correlation (2D HETCOR) showed that distinguished C4 chemical shifts correlates with the same aliphatic protons. The short-range ordering can be assigned to C4/C6 signals on 13C CPMAS and, for our case, the deconvolution procedure between disordered and ordered phases revealed increasing crystallinity with DA¯, as confirmed by SVD multivariate analysis. This work extended the knowledge regarding the use of 13C CPMAS technique to predict the crystallinity of chitosans without the use of amorphous standards.

3.
J Sci Food Agric ; 100(6): 2321-2326, 2020 Apr.
Article in English | MEDLINE | ID: mdl-31821568

ABSTRACT

Edible kernels have been popular food items since ancient times. Although in-shell nuts are naturally protected and relatively shelf stable, convenience demands require their commercialization in shelled form. However, whereas shelled kernels are more convenient, they are more exposed to oxygen, and thus more susceptible to oxidative rancidity and loss of crunchiness, which negatively affect the product acceptability. In this review, we discuss the role of edible coatings in extending stability of edible kernels, which is an opportunity to be better explored by the industry. The discussion also includes the role of antioxidants in the context of active coatings. Finally, future prospects and research challenges are addressed. © 2019 Society of Chemical Industry.


Subject(s)
Edible Films , Nuts , Seeds , Antioxidants , Food Handling/methods , Food Preservation/methods , Lipids/chemistry , Oxidation-Reduction
4.
Ciênc. rural (Online) ; 49(10): e20190310, 2019. tab, graf
Article in English | LILACS | ID: biblio-1045253

ABSTRACT

ABSTRACT: During the shelf-life of fresh meat, physical, chemical, microbiological, and sensory changes may occur. To avoid such changes, the combination of vacuum-packaging and use of edible coatings make a good strategy. This study aimed to evaluate the physicochemical characteristics of vacuum-packaged lamb meat combined with different zein-based edible coatings containing different vegetable oils (pink pepper, rosemary, olive oil, and the combinations of olive oil + pink pepper or rosemary), stored at 5 ± 1 °C. Parameters including pH, instrumental color, water holding capacity (WHC), shear force, and thiobarbituric acid reactive substances (TBARS) were analyzed every seven days, for 29 days. Significant differences (P<0.05) were observed in coating effects and storage time. The combination of olive oil and pepper oil (OLPP) exhibited higher color stability, while the coatings containing rosemary (RO), rosemary and olive oil (OLRO), and pink pepper oil (PP) exhibited the highest oxidative stability in 29 days. The pH, WHC, and shear force parameters did not appear to have been affected by the coatings. In summary, as appearance is an important purchasing factor, the coating containing olive oil and pink pepper oil is very promising as an alternative for maintaining vacuum-packaged lamb meat quality.


RESUMO: Durante a vida de prateleira da carne fresca podem ocorrer mudanças físico-químicas, microbiológicas e sensoriais indesejadas. Para evitar tais mudanças a combinação da embalagem tradicional à vácuo com revestimentos comestíveis é uma alternativa. O objetivo deste estudo foi avaliar o efeito do uso de diferentes revestimentos comestíveis à base de zeínas em combinação com diferentes óleos vegetais (óleos de: pimenta rosa, alecrim, azeite e combinação de azeite + óleo de pimenta rosa ou alecrim) nas características fisico-químicas da carne ovina, embalada à vácuo e armazenada à temperatura 5±1 °C. Foram realizadas análises de pH, cor instrumental, capacidade de retenção de água (CRA), força de cisalhamento, substâncias reativas ao ácido tiobarbitúrico (TBARS) a cada sete dias, no período de 29 dias. Foram observadas diferenças significativas (P<0,05) para o efeito de revestimentos e o tempo de armazenamento. A combinação de azeite mais óleo de pimenta (OLPP), apresentou maior estabilidade de cor, enquanto que os revestimentos contendo alecrim (RO), alecrim mais azeite (OLRO) e óleo de pimenta (PP) foram os que apresentaram maior estabilidade oxidativa no período de 29 dias. Os parâmetros pH, CRA e força de cisalhamento não parecem ter sido afetados pelos revestimentos. Tendo em vista que aparência é um importante fator de compra, o revestimento contendo azeite e óleo de pimenta rosa foi o mais promissor para ser utilizado na manutenção da qualidade de carne ovina.

5.
J Photochem Photobiol B ; 187: 41-47, 2018 Oct.
Article in English | MEDLINE | ID: mdl-30098521

ABSTRACT

OBJECTIVE: Mitochondrial dysfunction has been associated with the development of diabetes mellitus which is characterized by disorders of collagen production and impaired wound healing. This study analyzed the effects of photobiomodulation (PBM) mediated by laser and light-emitting diode (LED) on the production and organization of collagen fibers in an excisional wound in an animal model of diabetes, and the correlation with inflammation and mitochondrial dynamics. METHODS: Twenty Wistar rats were randomized into 4 groups of 5 animals. Groups: (SHAM) a control non-diabetic wounded group with no treatment; (DC) a diabetic wounded group with no treatment; (DLASER) a diabetic wounded group irradiated by 904 nm pulsed laser (40 mW, 9500 Hz, 1 min, 2.4 J); (DLED) a diabetic wounded group irradiated by continuous wave LED 850 nm (48 mW, 22 s, 1.0 J). Diabetes was induced by injection with streptozotocin (70 mg/kg). PBM was carried out daily for 5 days followed by sacrifice and tissue removal. RESULTS: Collagen fibers in diabetic wounded skin were increased by DLASER but not by DLED. Both groups showed increased blood vessels by atomic force microscopy. Vascular endothelial growth factor (VEGF) was higher and cyclooxygenase (COX2) was lower in the DLED group. Mitochondrial fusion was higher and mitochondrial fusion was lower in DLED compared to DLASER. CONCLUSION: Differences observed between DLASER and DLED may be due to the pulsed laser and CW LED, and to the higher dose of laser. Regulation of mitochondrial homeostasis may be an important mechanism for PBM effects in diabetes.


Subject(s)
Collagen/metabolism , Lasers , Light , Mitochondrial Dynamics/radiation effects , Animals , Cyclooxygenase 2/metabolism , Diabetes Mellitus, Experimental/chemically induced , Diabetes Mellitus, Experimental/pathology , Disease Models, Animal , GTP Phosphohydrolases , Male , Membrane Proteins/metabolism , Microscopy, Atomic Force , Mitochondrial Proteins/metabolism , Rats , Rats, Wistar , Skin/metabolism , Skin/pathology , Skin/radiation effects , Vascular Endothelial Growth Factor A/metabolism , Wound Healing/radiation effects
6.
Anal Bioanal Chem ; 408(14): 3875-9, 2016 05.
Article in English | MEDLINE | ID: mdl-27068694

ABSTRACT

High-resolution (13)C solid-state NMR stands out as one of the most promising techniques to solve the structure of insoluble proteins featuring biological and technological importance. The simplest nuclear magnetic resonance (NMR) spectroscopy method to quantify the secondary structure of proteins uses the areas of carbonyl and alpha carbon peaks. The quantification obtained by fitting procedures depends on the assignment of the peaks to the structure, type of line shape, number of peaks to be used, and other parameters that are set by the operator. In this paper, we demonstrate that the analysis of (13)C NMR spectra by a pattern recognition method-based on the singular value decomposition (SVD) regression, which does not depend on the operator-shows higher correlation coefficients for α-helix and ß-sheet (0.96 and 0.91, respectively) than Fourier transform infrared spectroscopy (FTIR) method. Therefore, the use of (13)C solid-state NMR spectra and SVD is a simple and reliable method for quantifying the secondary structures of insoluble proteins in solid-state.


Subject(s)
Carbon-13 Magnetic Resonance Spectroscopy/methods , Carbon Isotopes , Protein Structure, Secondary , Spectroscopy, Fourier Transform Infrared
7.
Braz. j. microbiol ; 43(1)Jan.-Mar. 2012.
Article in English | LILACS-Express | LILACS, VETINDEX | ID: biblio-1469577

ABSTRACT

Atomic Force Microscopy (AFM) can be used to obtain high-resolution topographical images of bacteria revealing surface details and cell integrity. During scanning however, the interactions between the AFM probe and the membrane results in distortion of the images. Such distortions or artifacts are the result of geometrical effects related to bacterial cell height, specimen curvature and the AFM probe geometry. The most common artifact in imaging is surface broadening, what can lead to errors in bacterial sizing. Several methods of correction have been proposed to compensate for these artifacts and in this study we describe a simple geometric model for the interaction between the tip (a pyramidal shaped AFM probe) and the bacterium (Escherichia coli JM-109 strain) to minimize the enlarging effect. Approaches to bacteria immobilization and examples of AFM images analysis are also described.

8.
Braz. j. microbiol ; 43(1): 341-347, Jan.-Mar. 2012. ilus, tab
Article in English | LILACS | ID: lil-622822

ABSTRACT

Atomic Force Microscopy (AFM) can be used to obtain high-resolution topographical images of bacteria revealing surface details and cell integrity. During scanning however, the interactions between the AFM probe and the membrane results in distortion of the images. Such distortions or artifacts are the result of geometrical effects related to bacterial cell height, specimen curvature and the AFM probe geometry. The most common artifact in imaging is surface broadening, what can lead to errors in bacterial sizing. Several methods of correction have been proposed to compensate for these artifacts and in this study we describe a simple geometric model for the interaction between the tip (a pyramidal shaped AFM probe) and the bacterium (Escherichia coli JM-109 strain) to minimize the enlarging effect. Approaches to bacteria immobilization and examples of AFM images analysis are also described.


Subject(s)
Cell Size , Escherichia coli , Microscopy, Atomic Force/methods , Optimization of Sanitary Sewer Network
9.
Braz. arch. biol. technol ; 48(4): 667-674, July 2005. ilus
Article in English | LILACS | ID: lil-410064

ABSTRACT

Um aspecto limitante a plena interpretação de imagens geradas por microscopia de força atômica é a interação entre a superfie varrida e ponta de varredura do sistema gerando artefatos de imagens. Para a identificação desses artefatos, propomos neste texto, um algoritmo simples capaz de assinalar esse tipo de irregularidade de imagem. A medida tem por princípio a identificação de ângulos similares formados entre dois pontos sobre a espécie varrida. O potencial de aplicação do método proposto é aqui ilustrado sobre um filme de polissacarídeo quitosana. As imagens geradas são comparadas entre si, indicando regiões de artefatos típicos gerados pela ponta de varredura. Este algoritmo apresenta-se como uma ferramenta útil a cientistas e usuários, permitindo a separação de aspectos reais e artificiais, que são fundamentais para uma melhor caracterização e medida.

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