联用技术应用于生物分子中金属和类金属的形态分析

本文依据最近有关联用技术应用于生物样品中痕量金属和类金属形态分析的报道，扼要介绍高效液相色谱（HPLC）和毛细管电泳（CE）与电感耦合等离子质谱（ICP－MS）和电喷雾离子化质谱（ESI－MS）联用技术在砷、硒和镉等元素的形态分析中的应用。体积排阻色谱（SEC）与ICP－MS在线联用最常用的初步筛选未知试样中大分子化合物的方法。但由于SEC的分辨率差，需要应用另一种色谱法，如离子交换色谱法（IEC）或反相色谱法（RP－HPLC）分离以保证分离信号的纯度。在无标准可利用的情况下，电喷雾串联质谱（ES－MS／MS）是用以表征化合物的最佳手段。毛细管区带电泳（CZE）与ICP－MS联用是形态分析的有用工具。分析中需要注意的问题是避免沾污和防止在分离过程中蛋白质的分解。目前，由于缺少标准和参考物质，联用技术主要应用于寻找新的金属物 种，而并非测定已知化合物。需要解决的难题是检测的信号是否属于某一特定的化合物以及该化合物的表征。

Speciation of Metals and Metalloids in Biomolecules by Hyphenated Techniques

This paper introduces briefly the analytical methods recently published in the literature on the speciation of arsenic, selenium and cadmium in biological samples using hyphenated techniques, HPLC ICP MS, HPLC ES MS/MS, and CE ES MS/MS The coupling SEC ICP MS is the most popular technique for the first screening of unknown sample in view of the presence of macro molecular species of element But due to its insufficient resolution, complementary chromatographic separations have to be carried out in order to guarantee the purity of the signal CZE ICP MS is a powerful tool in trace metal speciation In case standards and reference materials are not available, ES MS/MS is the best technique in the characterization of metal complexes During analysis care should be taken to avoid contamination of the sample and break up of the original metal protein bond during the separation process Due to lack of standards and reference materials, the application of hyphenated technique has been looking for new species rather than determining a known compound The difficult problems are whether a signal produced by a detector belongs to a particular compound and the identification of this compound