Kitazumi I, Nakashima Y, Himeno S
Department of Chemistry, Faculty of Science, Kobe University, Nada, Japan.
J Chromatogr A. 2001 Dec 21;939(1-2):123-9. doi: 10.1016/s0021-9673(01)01354-1.
A capillary electrophoretic (CE) method was developed for the sensitive determination of V(V) and V(IV). A Mo(VI)-P(V) reagent reacted with a mixture of trace amounts of V(V) and V(IV) to form the [P(V(V)Mo(11))O40]4- and [P(V(IV)Mo11)O40]5- complexes in 0.1 M monochloroacetate buffer (pH 2.2). Since the V-substituted Keggin anions possessed high molar absorptivities in the UV region and the peaks due to their migrations were well separated in the electropherogram, the pre-column complex formation reaction was applied to the simultaneous CE determination of V(V) and V(IV) with direct UV detection at 220 nm. The calibration curves were linear over two orders of magnitude with detection limits of 5 x 10(-7) M for V(V) and 2 x 10(-7) M for V(IV).
建立了一种毛细管电泳(CE)法用于灵敏测定V(V)和V(IV)。在0.1 M一氯乙酸缓冲液(pH 2.2)中,钼(VI)-磷(V)试剂与痕量V(V)和V(IV)的混合物反应,形成[P(V(V)Mo(11))O40]4-和[P(V(IV)Mo11)O40]5-配合物。由于V取代的Keggin阴离子在紫外区域具有高摩尔吸光系数,且其迁移产生的峰在电泳图中分离良好,因此采用柱前络合反应,通过在220 nm处直接紫外检测,对V(V)和V(IV)进行CE同时测定。校准曲线在两个数量级范围内呈线性,V(V)的检测限为5×10^(-7) M,V(IV)的检测限为2×10^(-7) M。