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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Filling the gap: Calibration of the low molar-mass range of cellulose in size exclusion chromatography with cello-oligomers
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Filling the gap: Calibration of the low molar-mass range of cellulose in size exclusion chromatography with cello-oligomers

机译：填补空白：使用纤维低聚物在尺寸排阻色谱法中校准纤维素的低摩尔质量范围

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摘要

Degraded celluloses are becoming increasingly important as part of product streams coming from various biorefinery scenarios. Analysis of the molar mass distribution of such fractions is a challenge, since neither established methods for mono- or disaccharides nor common methods for polysaccharide characterization cover the intermediate oligomer range appropriately. Size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS), the standard approach for celluloses, suffers from decreased scattering intensities in the lower-molar mass range. The limitation in the low-molecular range can, in principle, be overcome by calibration, but calibration standards for such "short" celluloses are either not readily available or structurally remote and thus questionable. In this paper, we present the calibration of a SEC system for the first time - with monodisperse cellooligomer standards up to about 3400 g mol(-1). These cellooligomers are "short-chain celluloses" and can be seen as the "true" standard compounds, by contrast to commonly used standards that are chemically different from cellulose, such as pullulan, dextran, polystyrene, or poly(methyl methacrylate). The calibration is compared against those commercial standards and correction factors are calculated. Calibrations with non-cellulose standards can now be adjusted to yield better fitting results, and data already available can be corrected retrospectively. (C) 2016 Elsevier B.V. All rights reserved.
机译：随着来自各种生物精炼厂的产品流的一部分，降解纤维素变得越来越重要。此类馏分的摩尔质量分布分析是一个挑战，因为既没有建立单糖或二糖的方法，也没有常用的多糖表征方法适当地涵盖了中间低聚物的范围。具有多角度激光散射（MALLS）的尺寸排阻色谱（SEC）是纤维素的标准方法，其在低摩尔质量范围内散射强度降低。原则上可以通过校准来克服低分子范围的限制，但是这种“短”纤维素的校准标准要么不容易获得，要么结构上遥不可及，因此值得商question。在本文中，我们首次展示了SEC系统的校准-单分散纤维素低聚物标准品的标准浓度约为3400 g mol（-1）。这些纤维素低聚物是“短链纤维素”，并且与化学上不同于纤维素的常用标准物（例如支链淀粉，葡聚糖，聚苯乙烯或聚甲基丙烯酸甲酯）相比，可以视为“真正的”标准化合物。将校准与那些商业标准进行比较，并计算校正因子。现在可以调整非纤维素标准品的校准，以产生更好的拟合结果，并且可以追溯地校正已经可用的数据。 （C）2016 Elsevier B.V.保留所有权利。

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