Otimização e validação de uma metodologia analítica para a determinação de produtos da conversão da celulose

Abstract

Due to high global energy demand and a concern for environmental preservation, a renewable energy source is becoming a very important strategy. In this sense, a cellulose is one of the most abundant and promising renewable resources, as its treatment by hydrolysis reaction are obtained biofuels and inputs of great industrial interest, such as: hydroxymethylfurfural (HMF), dihydroxyacetone (DHA), pyruvatedehyde, glyceraldehyde Acetic, formic, lactic and levulic acids. Therefore, the present work proposes an optimization and validation of an analytical methodology in the technique of high performance liquid chromatography (HPLC) for the determination of cellulose conversion products. The optimization of the proposed method was evaluated in a univariate and multivariate fashion. In the HPLC-optimized method, a cation exchange column, a solution of H 2 SO 4, was used as mobile phase with pH = 1.41, column temperature and detector of 42 ° C and 30 ° C respectively, flow of 0.9 mL / Min and total analysis time of 25.40 minutes. 10 analytical standards (glucose, fructose, glyceraldehyde, pyruvate, lactic acid, dihydroxyacetone, formic acid, acetic acid, levulinic acid and HMF) were used for this study. The HPLC method was validated by parameter selection, selectivity, linearity, limit of detection and limit of quantification, precision (repeatability, intermediate precision, instrumental accuracy), accuracy and robustness. These have been taken into consideration both the area and the height of the peaks. Analytical curves showed correlation coefficient ≥ 0.9972. The proposed methodology proved to be sensitive and accurate for a range of 5 to 500 μg / mL. In the instrumental precision, intermediate accuracy and repeatability values of CV ≤ 6,33% were obtained. Accuracy offers assessment methods from 90.58 to 106.87%, the proposed method is robust only for small variations of pH (± 1) and temperature (± 5) for dihydroxyacetone, glucose and pyruvate, which can be explained by the high temperature and pH values.