Confirmation of vanadium complex formation using electrospray mass spectrometry and determination of vanadium speciation by sample stacking capillary electrophoresis
Confirmation of vanadium complex formation using electrospray mass spectrometry and determination of vanadium speciation by sample stacking capillary electrophoresis
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DOI：
10.1016/j.aca.2006.12.008
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发表时间：
2007-02-28
影响因子：
6.2
通讯作者：
Naidu, Ravendra
中科院分区：
文献类型：
--
作者：
Chen, ZuLiang;Owens, Gary;Naidu, Ravendra
采用毛细管区带电泳-紫外检测法测定钒的形态。研究了次氮基三乙酸（NTA）、羟乙基乙二胺三乙酸（HEDTA）、乙二胺四乙酸（EDTA）、二乙烯三胺五乙酸（DTPA）、乙二醇双（2-氨基乙基醚）四乙酸（EGTA）和2，6-吡啶二甲酸（PDCA）等配体与钒形成稳定的阴离子配合物的情况。在所有研究的配体中，HEDTA是最合适的配体，因为它在合理的迁移时间内给出了最大的UV响应。电喷雾质谱（ES-MS）用于确认溶液中[VO 2（HEDTA）]（2-）和[VO（HEDTA）]（1-）的形成。含25 mM磷酸盐，0.25 mM十四烷基三甲基溴化铵（TTAB）在pH 5.5的电解质是最佳的分离这些阴离子钒络合物。样品堆积技术，包括大体积样品堆积（LVSS）和现场放大样品注射（FASI），进行了测试，以提高灵敏度。使用FASI获得最佳灵敏度，对于[VO 2（HEDTA）]（2-），检测限为0.001 μ M，相当于0.4 μ g L-1，对于[VO（HEDTA）]（1-），检测限为0.01 μ M，相当于3.4 μ g L-1。使用地下水样品证明了该方法用于V（IV）和V（V）形态的实用性。(c)2006 Elsevier B. V.保留所有权利。
Capillary zone electrophoresis (CZE) with UV detection was used to determine vanadium species. Nitrilotriacetic acid (NTA), hydroxyethylethylenediaminetriacetic acid (HEDTA), ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DTPA), ethylene glycol-bis(2-aminoethylether)-tetraacetic acid (EGTA) and 2,6-pyridinedicarboxylic acid (PDCA) were investigated to determine whether these ligands formed stable anionic complexes with vanadium. Of all the ligands studied HEDTA was the most suitable ligand because it gave the largest UV response with reasonable migration time. Electrospray mass spectrometry (ES-MS) was used to confirm the formation of [VO2(HEDTA)](2-) and [VO(HEDTA)](1-) in solution. An electrolyte containing 25 mM phosphate, 0.25 mM tetradecyltrimethylammonium bromide (TTAB) at pH 5.5 was optimum for the separation of these anionic vanadium complexes. Sample stacking techniques, including large-volume sample stacking (LVSS) and field-amplified sample injection (FASI), were tested to improve the sensitivity. Best sensitivity was obtained using FASI, with detection limits of 0.001 mu M, equivalent to 0.4 mu g L-1, for [VO2(HEDTA)](2-) and 0.01 mu M, equivalent to 3.4 mu g L-1 for [VO(HEDTA)](1-). The utility of the method for the speciation of V(IV) and V(V) was demonstrated using ground water samples. (c) 2006 Elsevier B.V. All rights reserved.