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无需预先水解的糖苷的气相色谱-质谱测定法。

Gas chromatographic-mass spectrometric determination of glycosides without prior hydrolysis.

作者信息

Isidorov Valery A, Nazaruk Jolanta

机构信息

Forest Faculty, Białystok University of Technology, 17-200 Hajnówka, Poland.

Medical University of Białystok, 15-089 Białystok, Poland.

出版信息

J Chromatogr A. 2017 Oct 27;1521:161-166. doi: 10.1016/j.chroma.2017.09.033. Epub 2017 Sep 18.

DOI:10.1016/j.chroma.2017.09.033
PMID:28941807
Abstract

The article presents for the first time the linear temperature programmed retention indices on a column with stationary phases of 5% phenylpolydimethyl silicone and the mass spectra of trimethylsilyl (TMS) derivatives of 71 glycosides (both commercial preparations and compounds extracted from plant tissues) which were not characterized earlier by these parameters. Converted to their TMS derivatives, the glycosides were thermally stable: they exhibited single peaks on their chromatograms without products of thermal decomposition. Therefore this work demonstrates the suitability of high resolution-high temperature gas chromatography (HR-HT/GC) to analyse different groups of glycosides including compounds with disaccharide moieties without the necessity of their hydrolyses. Since a limited number of commercial and plant-isolated glycosides were available, an attempt was made to assess their retention indices using the known "structure-retention relationships" approach. It was demonstrated that the retention indices of silanised glycosides and their aglycones were characterized by a linear dependence.

摘要

本文首次展示了在涂有5%苯基聚二甲基硅氧烷固定相的色谱柱上的线性程序升温保留指数,以及71种糖苷(包括市售制剂和从植物组织中提取的化合物)的三甲基硅烷基(TMS)衍生物的质谱,这些糖苷此前尚未通过这些参数进行表征。转化为TMS衍生物后,糖苷具有热稳定性:它们在色谱图上呈现单峰,没有热分解产物。因此,这项工作证明了高分辨率-高温气相色谱法(HR-HT/GC)适用于分析不同组的糖苷,包括具有二糖部分的化合物,而无需对其进行水解。由于可用的市售和植物分离的糖苷数量有限,尝试使用已知的“结构-保留关系”方法评估它们的保留指数。结果表明,硅烷化糖苷及其苷元的保留指数具有线性相关性。

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