Development and validation of analytical method for mono, di and triacetin analysis by HPLC/UV–Vis/DAD detection with 13C NMR identification

• Main Authors: Jadiete T.S. Gomes, Jackson H.S. Santos, Cesar A.M. Abreu, Eliane B.M. Medeiros, Lucas C.D. Coelho, Rui P.V. Faria, Alírio E. Rodrigues, Nelson M. Lima Filho
• Format: Article
• Language: English
• Published: Elsevier 2020-01-01
• Series: Results in Chemistry
• Subjects: HPLC; DAD; Quantitative characterization; Validation; Glycerol acetates
• Online Access: http://www.sciencedirect.com/science/article/pii/S2211715620300412

An analytical method was developed using high performance liquid chromatography with matrix of UV-VIS diodes to quantify mono, di and triacetin obtained from the acetylation of glycerol with acetic anhydride catalyzed by sodium acetate. The separation and validation of the method were performed with a C18 reverse phase column, using a mobile phase with centesimal composition in volumes of 59.6:0.4:40, corresponding to acetonitrile and dichloromethane with ultrapure water, respectively. Both the column and the detector were at 30 °C and the flow rate of the mobile phase was 0.5 mL min−1. As a complementary methodology, quick identifications were performed by 13C NMR of monoacetin, diacetin, triacetin and glycerol using the solvent DMSO-d6. The analytical curves obtained showed a good correlation coefficient (R2 ≥ 0.99) within the assessed concentration range. The method proved to be robust and accurate for the quantitative characterization of these acetates, when the correct wavelength was used (245 nm).