Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
7610046 | Journal of Chromatography A | 2016 | 7 Pages |
Abstract
A standard-free and sensitive method was developed for analysis of sucrose acetates in a crude 6-O-acetyl sucrose (S-6-a) product by on-line hydrolysis-high-performance liquid chromatography with pulsed amperometric detection (PAD). Sucrose, three regio-isomers of acetyl sucrose and five regio-isomers of diacetyl sucrose were separated on a C18 column using 3% (v/v) acetonitrile in water as eluent within 25 min. After purification with LC followed by semi-preparative HPLC, their chemical structures were identified by 1D, 2D NMR and LC-MS. Moreover, quantification of those regio-isomers was achieved by on-line alkaline hydrolysis to liberate sucrose using a post-column delivery system, and then detected by PAD for indirect estimation of the sucrose acetate content. Under optimal conditions, the linear ranges were from 0.03 to 150 μmol Lâ1 for sucrose corresponding to sucrose acetates with coefficient of determination as 0.9997 and detection limit as 0.01 μmol Lâ1 (S/N = 3). Good repeatability was obtained (RSD < 3%, n = 6). Furthermore, this method has been successfully applied to the analysis of sucrose and sucrose acetates in a crude S-6-a product during synthesis, purification and structure elucidation studies. The recoveries were from 94.89% to 102.31% for sucrose and sucrose acetates.
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Authors
Wenwu Yan, Nani Wang, Peimin Zhang, Jiajie Zhang, Shuchao Wu, Yan Zhu,