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%).