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Development and validation of analytical method for mono, di and triacetin analysis by HPLC/UV–Vis/DAD detection with 13C NMR identification
Results in Chemistry Pub Date : 2020-07-15 , DOI: 10.1016/j.rechem.2020.100063
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

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).



中文翻译:

HPLC / UV-Vis / DAD检测和13 C NMR鉴定的单,双和三醋精分析方法的开发和验证

开发了一种使用高效液相色谱和UV-VIS二极管矩阵的分析方法,以定量测定乙酸钠催化乙酸酐对甘油的乙酰化作用而获得的甘油单酯,甘油二酯和甘油三酯。该方法的分离和验证是使用C18反相柱进行的,使用百分组成为59.6:0.4:40的流动相,分别对应于超纯水的乙腈和二氯甲烷。色谱柱和检测器均处于30°C,流动相的流速为0.5 mL min -1。作为补充方法,使用溶剂DMSO- d 6通过单乙酸甘油酯,双乙酸甘油酯,甘油三乙酸甘油酯和甘油的13 C NMR快速鉴定。该分析曲线获得显示出良好的相关系数(R 2 被评估的浓度范围内≥0.99)。当使用正确的波长(245 nm)时,该方法被证明对这些乙酸盐的定量表征是可靠且准确的。

更新日期:2020-07-15
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