Sjövall Peter, Lausmaa Jukka, Johansson Bo-Lennart, Andersson Mikael
Department of Chemistry and Materials Technology, SP Swedish National Testing and Research Institute, P.O. Box 857, SE-50115 Borås, Sweden, and Research and Development, Amersham Biosciences AB, SE-751 84 Uppsala, Sweden.
Anal Chem. 2004 Apr 1;76(7):1857-64. doi: 10.1021/ac035457g.
The surface chemical structure of two raw materials (agarose and dextran) and four base matrixes used in the manufacture of chromatography media were analyzed using time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results show that the small differences in molecular structure between these materials result in significant differences in the TOF-SIMS spectra and that these differences can be identified and quantified using either of two different approaches. In a novel approach, fragment ion distributions were extracted from the TOF-SIMS spectra for each material, providing an immediate and systematic overview of the spectral features. Difference fragment distributions were used to highlight spectral differences between the materials. The results of the fragment ion distribution analysis, in terms of identification and quantification of spectral variations between different materials, were found to be in agreement with the results from a principal component analysis using the same set of data. Both methods were found capable of (i) distinguishing between agarose and dextran and (ii) detecting and quantifying the degree of cross-linking present in the four base matrix materials. In addition, using a deuterated chemical cross-linker, it was possible to identify spectral features specifically connected to the cross-link molecular structure.
使用飞行时间二次离子质谱法(TOF-SIMS)分析了用于制造色谱介质的两种原材料(琼脂糖和葡聚糖)以及四种基础基质的表面化学结构。结果表明,这些材料之间分子结构的微小差异导致了TOF-SIMS光谱的显著差异,并且可以使用两种不同方法中的任何一种来识别和量化这些差异。在一种新颖的方法中,从每种材料的TOF-SIMS光谱中提取碎片离子分布,从而提供光谱特征的即时和系统概述。差异碎片分布用于突出材料之间的光谱差异。发现碎片离子分布分析在识别和量化不同材料之间光谱变化方面的结果与使用同一组数据进行主成分分析的结果一致。两种方法都能够(i)区分琼脂糖和葡聚糖,以及(ii)检测和量化四种基础基质材料中存在的交联程度。此外,使用氘代化学交联剂,可以识别与交联分子结构特异性相关的光谱特征。