Klampfl C W, Buchberger W
Department of Analytical Chemistry, Johannes Kepler-University Linz, Austria.
Electrophoresis. 2001 Aug;22(13):2737-42. doi: 10.1002/1522-2683(200108)22:13<2737::AID-ELPS2737>3.0.CO;2-Z.
A method for the determination of underivatized carbohydrates using capillary electrophoresis (CE) with detection by electrospray ionization-mass spectrometry (ESI-MS) presented. Highly alkaline carrier electrolytes based on volatile organic bases like is diethylamine (DEA) combined with MS detection in the negativ-ion mode proved to be the optimum solution for the separation and detection of these analytes. Optimization of the carrier electrolyte composition has been performed with respect to its pH, ionic strength as well as the addition of an organic modifier. The influence of the DEA concentration in the sheath liquid on parameters like peak shapes or signal-to-noise (S/N) ratios was also investigated. Limits of detection (LOD) were in the range of 0.5-3.0 mgL(-1) and calibration was linear over an order of magnitude for almost all solutes investigated. Finally, the applicability of this method for the analysis of real samples was demonstrated with wine samples.
介绍了一种使用毛细管电泳（CE）结合电喷雾电离质谱（ESI-MS）检测来测定未衍生化碳水化合物的方法。基于挥发性有机碱（如二乙胺，DEA）的高碱性载体电解质与负离子模式下的质谱检测相结合，被证明是分离和检测这些分析物的最佳解决方案。已针对载体电解质的pH值、离子强度以及有机改性剂的添加对其组成进行了优化。还研究了鞘液中DEA浓度对峰形或信噪比（S/N）等参数的影响。检测限（LOD）在0.5 - 3.0 mgL(-1)范围内，几乎所有研究的溶质在校准范围内呈线性关系，线性范围达一个数量级。最后，用葡萄酒样品证明了该方法在实际样品分析中的适用性。
