Determination of the substitution patterns of cellulose methyl ethers by HPLC and GLC-comparison of methods

Determination of the substitution patterns of cellulose methyl ethers by HPLC and GLC-comparison of methods
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通过 HPLC 和 GLC 测定纤维素甲基醚的取代模式 - 方法比较

DOI:
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发表时间:
1992
期刊:
影响因子:
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通讯作者:
D. Klemm
D. Klemm
中科院分区:
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文献类型:
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作者:
U. Erler;P. Mischnick;A. Stein;D. Klemm

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通过水解和分离所得的部分甲基化葡萄糖,无需进一步衍生化,通过高效液相色谱法测定了甲基纤维素以及thexyldimethylsilylcellulose在全甲基化后的取代模式。在胺改性的硅胶柱上,溶质被分离成葡萄糖、2,3,6-三-O-甲基葡萄糖以及单-O-甲基-和二-O-甲基葡萄糖。在反相柱上进行的色谱分析能够鉴别单-O-甲基-和二-O-甲基葡萄糖。以这种方式,可以测定纤维素衍生物的平均取代度和取代模式。将结果与通过标准甲基化分析(包括g.l.c.- M.S.证明了所用方法的正确性。
SummaryThe substitution patterns of methyl cellulose as well as of a thexyldimethylsilyl cellulose after permethylation were determined by hydrolysis and separation of the resulting partially methylated glucoses without further derivatization by h.p.l.c.. On an amine-modified silica column the solutes get separated into glucose, 2,3,6-tri-O-methyl glucose and the groups of mono-O-methyl-and di-O-methyl glucoses. A chromatographic run on a reversed-phase column enables the identification of the single mono-O-methyl- and di-O-methyl glucoses. In this way, a determination of both the average degree of substitution and the substitution pattern of cellulose derivatives is possible. Comparison of the results with those obtained by standard methylation analysis including g.l.c.-m.s. proves the correctnes of the method employed.
通过还原裂解法分析部分甲基化或乙基化纤维素中 O-甲基或 O-乙基的取代位置。
DOI: 10.1016/0008-6215(88)85046-8
发表时间: 1988
影响因子: 3.1
作者:
D'Ambra,AJ;Rice,MJ;Zeller,SG;Gruber,PR;Gray,GR
通讯作者: Gray,GR