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通过阴离子交换高效液相色谱-电感耦合等离子体发射光谱法对柠檬酸铝和其他带负电荷的铝配合物进行物种形成分析的可能性。

Possibilities for speciation of Al-citrate and other negatively charged Al complexes by anion-exchange FPLC-ICP-AES.

作者信息

Bantan T, Milacic R, Pihlar B

机构信息

Department of Environmental Sciences, Jozef Stefan Institute, Jamova 39, 1000 Ljubljana, Slovenia.

出版信息

Talanta. 1998 May;46(1):227-35. doi: 10.1016/s0039-9140(97)00282-8.

Abstract

An anion-exchange fast protein liquid chromatographic-inductively coupled plasma atomic emission spectrometric procedure (FPLC-ICP-AES) was developed for speciation of Al-citrate and other negatively charged Al complexes. FPLC separations were carried out on a Mono Q HR 5/5 strong anion-exchange FPLC column over a pH range from 3.5 to 11.0. An aqueous-NaNO(3) (4 mol dm(-3)) linear gradient elution was applied over 10 min for separation of a particular Al species. The separated Al species were determined in 0.5 cm(3) eluate fractions ;off line' by ICP-AES. Under optimal analytical procedures Al-citrate was separated from Al-oxalate and Al-EDTA in a neutral pH range. Good reproducibility of the FPLC-ICP-AES procedure was obtained for determination of a particular Al species at optimal measurement conditions (RSD +/-2%). Al(3+) and neutral Al-citrate species were strongly adsorbed on the column resin and did not interfere with the separation of negatively charged Al complexes. Al(OH)(4)(-) species were separated from Al-citrate in an alkaline pH region, but quantitatively determined only at a pH of 11.0. The distribution of Al species over a pH range from 3.5 to 11.0 agreed with the reported calculated data. The limit of detection (3sigma basis) for separated Al species was 0.1 mug cm(-3).

摘要

开发了一种阴离子交换快速蛋白质液相色谱-电感耦合等离子体原子发射光谱法(FPLC-ICP-AES),用于柠檬酸铝和其他带负电荷的铝配合物的形态分析。FPLC分离在Mono Q HR 5/5强阴离子交换FPLC柱上进行,pH范围为3.5至11.0。采用水-NaNO₃(4 mol dm⁻³)线性梯度洗脱,在10分钟内分离特定的铝物种。分离出的铝物种在0.5 cm³洗脱液馏分中离线通过ICP-AES测定。在最佳分析程序下,柠檬酸铝在中性pH范围内与草酸铝和铝-EDTA分离。在最佳测量条件下,FPLC-ICP-AES法测定特定铝物种具有良好的重现性(RSD±2%)。Al³⁺和中性柠檬酸铝物种强烈吸附在柱树脂上,不干扰带负电荷的铝配合物的分离。Al(OH)₄⁻物种在碱性pH区域与柠檬酸铝分离,但仅在pH为11.0时可定量测定。在3.5至11.0的pH范围内铝物种的分布与报道的计算数据一致。分离出的铝物种的检测限(基于3σ)为0.1 μg cm⁻³。

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