Improvement of an Analytical Method Based on HPLC With Refractive Index Detection for the Analysis of Glycerol Oxidation Products

Abstract

The optimized analytical methodology described herein is based on an ion exchange column and an H 3 PO 4 solution (pH 2.24) as the mobile phase, with a flow rate of 0.4 mL min-1 and refractive index detection (RID). On applying the methodology, it was possible to identify 7 products obtained from the oxidation of glycerol with an analysis time of 27 min. The developed method was validated through the evaluation of a series of analytical parameters. The results obtained were evaluated considering the peak area and peak height. The analytical curves showed a correlation coefficient of ≥ 0.986. The coefficient of variation values obtained were ≤ 3.60% for instrumental precision, ≤ 19.36% for intermediate precision in LOQ (1.25 µg mL-1) and ≤ 17.93% for repeatability in LOQ (1.25 µg mL-1) and different days. The limit of quantification established for all compounds was 1.25 μg mL-1 obtained through the parameters of the analytical curve. The accuracy of the method showed recovery values of 85.6 to 112.3% for real fortified sample at 3 concentration levels. Two different samples of glycerol oxidation products were applied to the validated methodology; one obtained from AuNP/SiO 2 as catalyst (conversion of 62.42%), and other using AuNP/MWCNT (conversion of 89.5%).

Electrocatalytic Conversion of Glycerol to Oxalate on Ni Oxide Nanoparticles-Modified Oxidized Multiwalled Carbon Nanotubes

“…Nevertheless, a significant challenge is the control of the GOR selectivity while simultaneously achieving high reaction rates and high conversions 24,25 since its various reaction pathways often lead to complex mixtures as the final product. 20,21,26 There is currently a limited number of studies reporting highly active GOR catalysts based on earth-abundant materials, 27−31 and even less demonstrating high selectivity toward value-added products. Among them, Ni-based catalysts seem to be promising candidates in terms of catalytic GOR performance, offering relatively low overpotentials and predominant selectivity toward formate.…”

“…Thus, new methods and technologies for oxalic acid production are rising, some involving electrosynthesis routes. , Hence, the electrochemical synthesis of oxalic acid via the GOR is of great interest for potential industrial applications. Nevertheless, a significant challenge is the control of the GOR selectivity while simultaneously achieving high reaction rates and high conversions , since its various reaction pathways often lead to complex mixtures as the final product. ,, There is currently a limited number of studies reporting highly active GOR catalysts based on earth-abundant materials, − and even less demonstrating high selectivity toward value-added products. Among them, Ni-based catalysts seem to be promising candidates in terms of catalytic GOR performance, offering relatively low overpotentials and predominant selectivity toward formate. ,, While some studies demonstrate the formation of C2 or C3 products, improved selectivity still represents a major challenge. − …”

A cellulose monolithic stir bar for sorptive extraction of glycerol from biodiesel

“…The proposed method shows lower detectability of other extraction methods with HPLC-RID analysis. 14,49,50…”

“…The proposed method shows lower detectability of other extraction methods with HPLC-RID analysis. 14,49,50 Analytical parameters of linearity, range, and sensitivity were obtained from the construction of analytical curves for glycerol. Fig.…”