Polyhedral oligomeric silsesquioxanes (POSSs) are a class of important hybrid inorganic/organic materials. When POSSs are used as the building block in polymerization, the materials show superior performance over their organic counterparts in many areas due to the special Si–O cage structure. However, the stereoisomers (cis, trans) of polyhedral oligomeric silsesquioxane (POSS) show some differences in improving polymer property and it is difficult to get the pure stereoisomer by synthesis. Therefore, a method is required to separate and purify the mixture of POSSs. In this study, the isomers of POSS compounds and the impurities were separated by ultra-high performance supercritical fluid chromatography coupled quadrupole time-of-flight mass spectrometry (UHPSFC-QTof MS). To separate the isomers of POSS, the crucial parameters of UHPSFC-QTof MS were investigated. Under the optimal conditions, the isomers of product and impurities were separated in 4 min. On account of exact mass measurement, some impurities were identified. This is the first study on the analysis of isomers of POSS using UHPSFC-QTof MS. Based on this analysis method, it is helpful to optimize the conditions of synthesis.

中文翻译：

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使用 UHPSFC-QTof MS 分析多面体低聚倍半硅氧烷化合物的立体异构体（顺式、反式）

多面体低聚倍半硅氧烷 (POSS) 是一类重要的无机/有机杂化材料。当 POSSs 用作聚合反应的构建块时，由于特殊的 Si-O 笼结构，该材料在许多领域表现出优于有机材料的性能。然而，多面体低聚倍半硅氧烷（POSS）的立体异构体（顺式、反式）在改善聚合物性能方面表现出一些差异，并且难以通过合成获得纯立体异构体。因此，需要一种方法来分离和纯化 POSS 的混合物。在本研究中，POSS 化合物的异构体和杂质通过超高效超临界流体色谱耦合四极杆飞行时间质谱 (UHPSFC-QTof MS) 进行分离。为了分离 POSS 的异构体，研究了 UHPSFC-QTof MS 的关键参数。在最佳条件下，产物的异构体和杂质在4分钟内分离。由于精确的质量测量，鉴定了一些杂质。这是使用 UHPSFC-QTof MS 分析 POSS 异构体的第一项研究。基于这种分析方法，有助于优化合成条件。