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Power of Ultra Performance Liquid Chromatography/Electrospray Ionization-MS Reconstructed Ion Chromatograms in the Characterization of Small Differences in Polymer Microstructure

机译:超高效液相色谱/电喷雾电离-S MS重建离子色谱图在聚合物微观结构小差异中的表征

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摘要

From simple homopolymers to functionalized, 3-dimensional structured copolymers, the complexity of polymeric materials has become more and more sophisticated. With new applications, for instance, in the semiconductor or pharmaceutical industry, the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isomeric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector but affect the properties of materials significantly. For a drug delivery system, for example, the degree of branching and branching distribution is crucial for the formation of micelles. Instead of a complicated, time-consuming, and/or expensive 2D-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, in this work, a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization (ESI) mass spectrometry is proposed. The online coupling allows the analysis of reconstructed ion chromatograms (RICs) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities. Although some microstructural heterogeneities like short chain branching can for large polymers be characterized with methods such as light scattering, for oligomers where the heterogeneities just start to form and their influence is at the maximum, they are inaccessible with these methods. It is also shown that with a proper calibration even quantitative information can be obtained. This method is suitable to detect small differences in, e.g., branching, 3D-structure, monomer sequence, or tacticity and could potentially be used in routine analysis to quickly determine deviations.
机译:从简单的均聚物从功能化,三维结构共聚物,聚合物材料的复杂性变得越来越复杂。例如,在半导体或制药行业中,具有新的应用,表征的要求随着所用聚合物的复杂性而上升。对于每个额外的分布,需要在分析中进行额外的维度。小型,通常在拓扑或微观结构中的异构性异质性通常不能简单地在色谱描绘或由任何常见的探测器分开,而是显着影响材料的性质。对于药物递送系统,例如,分支和支化分布的程度对于胶束形成至关重要。代替复杂,耗时和/或昂贵的2D色谱或离子迁移谱图(IMS)方法,也具有其限制,在这项工作中,使用尺寸排阻色谱(SEC)与电喷雾电离(建议ESI)质谱。在线耦合允许分析每种聚合度的重建离子色谱图(RIC)。虽然通常无法实现完全分离,但是衍生的保留时间和峰宽导致有关异质性存在和分散的信息。尽管具有短链支化可以用于大型聚合物的一些微观结构的异质性,但是对于诸如光散射的方法表征,用于低聚物,其中异质体刚刚开始形成并且它们的影响最大,它们与这些方法无法访问。还示出,可以获得适当的校准甚至可以获得定量信息。该方法适合于检测小差异,例如分支,3D结构,单体序列或术后,并且可能用于常规分析以快速确定偏差。

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  • 来源
    《Analytical chemistry》 |2018年第5期|共8页
  • 作者单位

    Bundesanstalt für Materialforschung und?prüfung (BAM) Richard-Willst?tter-Stra?e 11 12489 Berlin Germany;

    Bundesanstalt für Materialforschung und?prüfung (BAM) Richard-Willst?tter-Stra?e 11 12489 Berlin Germany;

    Bundesanstalt für Materialforschung und?prüfung (BAM) Richard-Willst?tter-Stra?e 11 12489 Berlin Germany;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 分析化学;
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