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 H3PO4 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/SiO2 as catalyst (conversion of 62.42%), and other using AuNP/MWCNT (conversion of 89.5%).

Keywords

• High-performance Liquid Chromatography
• ion exchange column
• glycerol oxidation
• analytical methodologies
• identification and quantification