Strong magnetoelectrolysis effect during electrochemical reaction monitored in situ by high-resolution NMR spectroscopy.

The strong effect of magnetic field on the electrochemical (EC) reduction of a diamagnetic species was monitored in situ in a 600 MHz (14 T) NMR spectrometer. Throughout EC-NMR experiments, the diamagnetic species is influenced by the Lorentz force (cross product of current density and magnetic field), which in turn acts on analyte transport and, as a result, enhances reaction rates. This phenomenon, known as magnetoelectrolysis, has not been considered in several in situ EC-NMR studies in solution, electron paramagnetic resonance (EC-EPR) spectroscopy, and magnetic resonance imaging (EC-MRI) involving the oxidation and reduction of organic compounds and lithium ion batteries. Recently, we have demonstrated the presence of this effect in the electroplating of a paramagnetic ion species by monitoring it in situ in a low-field (0.23 T) NMR spectrometer. In this report, a ca. five-fold enhancement in the electroreduction rate of benzoquinone was observed when the analyses were performed in situ in the NMR spectrometer. Therefore, this work has the objective of informing the scientific community that before every electrochemical reaction carried out in situ in NMR, EPR and MRI apparatuses, the influence of the magnetic field on the reactions must be evaluated, since it can alter the mechanism and kinetics of the reaction which, if not taken into account may lead to wrong interpretations of the data.

Metabolic fingerprint of Brazilian maize landraces silk (stigma/styles) using NMR spectroscopy and chemometric methods.

Aqueous extract from maize silks is used by traditional medicine for the treatment of several ailments, mainly related to the urinary system. This work focuses on the application of NMR spectroscopy and chemometric analysis for the determination of metabolic fingerprint and pattern recognition of silk extracts from seven maize landraces cultivated in southern Brazil. Principal component analysis (PCA) of the (1)H NMR data set showed clear discrimination among the maize varieties by PC1 and PC2, pointing out three distinct metabolic profiles. Target compounds analysis showed significant differences (p < 0.05) in the contents of protocatechuic acid, gallic acid, t-cinnamic acid, and anthocyanins, corroborating the discrimination of the genotypes in this study as revealed by PCA analysis. Thus the combination of (1)H NMR and PCA is a useful tool for the discrimination of maize silks in respect to their chemical composition, including rapid authentication of the raw material of current pharmacological interest.

Evaluation of biodiesel-diesel blends quality using 1H NMR and chemometrics.

In this work, the use of (1)H NMR spectroscopy and statistical approach to the evaluation of biodiesel-diesel blends quality is described. Forty-six mixtures of oil-diesel, biodiesel-diesel, and oil-biodiesel-diesel were analyzed by (1)H NMR and such data were employed to design four predictive models. Thirty-six mixtures were used in the calibration set and the others in the validation. The PCR and PLS models were evaluated through statistical parameters. Briefly, PLS and PCR models were suitable for the prediction of biodiesel and oil concentration in mineral diesel. Specially, in higher concentration the predicted values were quite similar to the real ones. This fact was evidenced by the low relative errors of high concentrated samples; this means that the prediction of low concentrated samples will probably show high deviation. Therefore, (1)H NMR-PLS and (1)H NMR-PCR methods are fairly useful for the quality control of biodiesel-diesel blends, particularly they are suitable for prediction of concentrations greater than 2%.