Determination of fat-soluble vitamins in vegetable oils through microwave-assisted high-performance liquid chromatography

In this manuscript, a study of the effect of microwave radiation on the high-performance liquid chromatography separation of tocopherols and vitamin K1 was conducted. The novelty of the application was the use of a relatively low polarity mobile phase in which the dielectric heating effect was minimized to evaluate the nonthermal effect of the microwave radiation over the separation process. Results obtained show that microwave-assisted high-performance liquid chromatography had a shorter analysis time from 31.5 to 13.3 min when the lowest microwave power was used. Moreover, narrower peaks were obtained; hence the separation was more efficient maintaining or even increasing the resolution between the peaks. This result confirms that the increase in mobile phase temperature is not the only variable for improving the separation process but also other nonthermal processes must intervene. Fluorescence detection demonstrated better signal-to-noise compared to photodiode arrayed detection mainly due to the independent effect of microwave pulses on the baseline noise, but photodiode array detection was finally chosen as it allowed a simultaneous detection of nonfluorescent compounds. Finally, a determination of the content of the vitamin E homologs was carried out in different vegetable oils. Results were coherent with those found in the literature.

Removal of BrO3 − from drinking water samples using newly developed agricultural waste-based activated carbon and its determination by ultra-performance liquid chromatography-mass spectrometry

Activated carbon was prepared from date pits via chemical activation with H3PO4. The effects of activating agent concentration and activation temperature on the yield and surface area were studied. The optimal activated carbon was prepared at 450 °C using 55 % H3PO4. The prepared activated carbon was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer, Emmett, and Teller (BET) surface area. The prepared date pit-based activated carbon (DAC) was used for the removal of bromate (BrO3 −). The concentration of BrO3 − was determined by ultra-performance liquid chromatography-mass tandem spectrometry (UPLC-MS/MS). The experimental equilibrium data for BrO3 − adsorption onto DAC was well fitted to the Langmuir isotherm model and showed maximum monolayer adsorption capacity of 25.64 mg g−1. The adsorption kinetics of BrO3 − adsorption was very well represented by the pseudo-first-order equation. The analytical application of DAC for the analysis of real water samples was studied with very promising results.

Enhanced electrocatalytic activity of Au@Cu core@shell nanoparticles towards CO2 reduction

The development of technologies for the recycling of carbon dioxide into carbon-containing fuels is one of the major challenges in sustainable energy research. Two of the main current limitations are the poor efficiency and fast deactivation of catalysts. Core–shell nanoparticles are promising candidates for enhancing challenging reactions. In this work, Au@Cu core–shell nanoparticles with well-defined surface structures were synthesized and evaluated as catalysts for the electrochemical reduction of carbon dioxide in neutral medium. The activation potential, the product distribution and the long term durability of this catalyst were assessed by electrochemical methods, on-line electrochemical mass spectrometry (OLEMS) and on-line high performance liquid chromatography. Our results show that the catalytic activity and the selectivity can be tweaked as a function of the thickness of Cu shells. We have observed that the Au cubic nanoparticles with 7–8 layers of copper present higher selectivity towards the formation of hydrogen and ethylene; on the other hand, we observed that Au cubic nanoparticles with more than 14 layers of Cu are more selective towards the formation of hydrogen and methane. A trend in the formation of the gaseous products can be also drawn. The H2 and CH4 formation increases with the number of Cu layers, while the formation of ethylene decreases. Formic acid was the only liquid species detected during CO2 reduction. Similar to the gaseous species, the formation of formic acid is strongly dependent on the number of Cu layers on the core@shell nanoparticles. The Au cubic nanoparticles with 7–8 layers of Cu showed the largest conversion of CO2 to formic acid at potentials higher than 0.8 V vs. RHE. The observed trends in reactivity and selectivity are linked to the catalyst composition, surface structure and strain/electronic effects.