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反相 C18 整体柱的柱制备重现性及其在生育酚同系物分离中的应用。

Repeatability in column preparation of a reversed-phase C18 monolith and its application to separation of tocopherol homologues.

机构信息

Flow Innovation-Research for Science and Technology Laboratories (FIRST Labs) Mahidol University, Rama VI Rd., Bangkok 10400, Thailand.

出版信息

Talanta. 2011 Jun 15;84(5):1374-8. doi: 10.1016/j.talanta.2011.03.083. Epub 2011 Apr 5.

DOI:10.1016/j.talanta.2011.03.083
PMID:21641454
Abstract

This work investigated the repeatability of column preparation for a reversed-phase C18 monolith, namely stearyl methacrylate-co-ethylene glycol dimethacrylate (SMA-EDMA). The columns were thermally polymerised using three commonly available heating devices (GC oven, hot air oven and water bath) and their chromatographic performance evaluated using micro-liquid chromatography for separation of five test compounds. Precision in terms of %RSD of retention times were 9.0, 6.5, and 12.5 using GC oven, hot air oven and water bath, respectively. Between-batch precision for the hot air oven (n=3 days) was less than 10.4% for retention time. The SMA-EDMA monolith was applied to the separation of tocopherol homologues by capillary electrochromatography. Usually tocopherol homologues cannot be completely separated by conventional reversed-phase C8- or C18-packed bed or C18-silica based monolithic columns. Polymer monolith has been shown to give remarkable selectivity towards the tocopherols compared to the conventional microparticulate phase and silica based monolith. Successful separation of the tocopherol isomers was achieved on the SMA-EDMA monolith without any column modification.

摘要

本工作研究了反相 C18 整体柱(即硬脂基甲基丙烯酸酯-乙二醇二甲基丙烯酸酯(SMA-EDMA))的柱制备重复性。使用三种常用的加热设备(GC 炉、热空气炉和水浴)对柱进行热聚合,并使用微液相色谱法评估其色谱性能,以分离五种测试化合物。使用 GC 炉、热空气炉和水浴时,保留时间的 RSD%精度分别为 9.0、6.5 和 12.5。热空气炉(n=3 天)的批间精密度小于 10.4%。SMA-EDMA 整体柱应用于通过胶束电动色谱法分离生育酚同系物。通常,生育酚同系物不能通过常规反相 C8 或 C18 填充床或 C18-硅胶基整体柱完全分离。与传统的微颗粒相和硅胶基整体柱相比,聚合物整体柱显示出对生育酚的显著选择性。无需对 SMA-EDMA 整体柱进行任何柱改性即可成功分离生育酚异构体。

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