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High‐resolution separation of homogeneous chitooligomers series from 2‐mers to 7‐mers by ion‐exchange chromatography
Author(s) -
Li Kecheng,
Liu Song,
Xing Ronge,
Yu Huahua,
Qin Yukun,
Li Rongfeng,
Li Pengcheng
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200935
Subject(s) - oligomer , polymerization , chemistry , degree of polymerization , glucosamine , resolution (logic) , hydrolysis , chromatography , ion chromatography , polymer chemistry , organic chemistry , polymer , computer science , artificial intelligence
Highly purified chitooligomers with single degree of polymerization are of significance for studying bioactivity of chitooligomers. However, there are few reports on high‐resolution preparative separation of chitooligomers, especially for those oligomers with degree of polymerization higher than 4. This study developed a high‐resolution chromatography for the preparative separation of a pure fully deacetylated chitooligomer series. A glucosamine oligomer mixture with low degree of polymerization was prepared by acid hydrolysis of a highly deacetylated chitosan. Then, six fractions were separated from the prepared oligomer mixture by ion‐exchange chromatography and analyzed by HPLC and ESI / MS , which primarily contained glucosamine dimers, trimers, tetramers, pentamers, hexamers, and heptamers, respectively, with chromatographic purities over 98% for dimers to hexamers and a purity of 93% for heptamers. The yields of a single round of separation were 75, 60, 60, 55, 35, and 20 mg for glucosamine dimers, trimers, tetramers, pentamers, hexamers, and heptamers, respectively. Furthermore, a chromatographic separation model for G lc N homomers was established. The capacity factor ( k ) of glucosamine oligomers and their degrees of polymerization ( DP s) exhibited a good correlation, ln k = 0.786 + 0.846 ln DP , ( R 2 = 0.997). Based on this equation, glucosamine octamers are expected to be separated by this system.