Pérez-Ruiz Tomás, Martínez-Lozano Carmen, García María Dolores
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, 30071 Murcia, Spain.
J Chromatogr A. 2007 Oct 26;1169(1-2):151-7. doi: 10.1016/j.chroma.2007.09.017. Epub 2007 Sep 14.
A simple, selective and sensitive method for the determination of aminopolycarboxylic acids [diethylenetriaminepentaacetic acid (DTPA), S,S-ethylenediamine N,N'-disuccinic acid (EDDS), ethylenediaminetetraacetate (EDTA) and nitrilotriacetate (NTA)] has been developed using high-performance liquid chromatography with chemiluminescence detection. The aminopolycarboxylic acids were separated on a C18 reversed-phase column with an aqueous sulfuric acid mobile phase at a pH lower than 1.5. The eluate was mixed with tris(2,2'-bipyridyl)ruthenium(III), which was on-line generated by photooxidation of the ruthenium(II) complex in the presence of peroxydisulfate, and the generated chemiluminescence was detected. Calibration graphs, based on standard solutions, were linear over the range 8x10(-9) to 4x10(-5) M. The detection limits at a signal-to-noise ratio of 3 ranged from 9x10(-10) to 8x10(-8) M. The relative standard deviations of intra- and inter-day precision were below 1.3% and 2.1%, respectively. This HPLC system was successfully applied to the determination of aminopolycarboxylic acids in three different types of water samples. The low pH of the mobile phase limits interference from metal ions in natural waters. When such interference occurs, a cation-exchange column can be used to suppress it. The lowest amounts measurable were: 75 pg for NTA, 0.7 ng for EDDS, 0.8 ng for DTPA and 12ng for EDTA. The method was also applied for the EDTA assay in canned foods.
已开发出一种简单、选择性好且灵敏的方法,用于测定氨基多羧酸[二乙三胺五乙酸(DTPA)、S,S-乙二胺-N,N'-二琥珀酸(EDDS)、乙二胺四乙酸(EDTA)和次氮基三乙酸(NTA)],该方法采用高效液相色谱-化学发光检测法。氨基多羧酸在C18反相柱上分离,流动相为pH低于1.5的硫酸水溶液。洗脱液与三(2,2'-联吡啶)钌(III)混合,后者在过二硫酸盐存在下通过钌(II)配合物的光氧化在线生成,然后检测产生的化学发光。基于标准溶液的校准曲线在8×10⁻⁹至4×10⁻⁵ M范围内呈线性。信噪比为3时的检测限为9×10⁻¹⁰至8×10⁻⁸ M。日内和日间精密度的相对标准偏差分别低于1.3%和2.1%。该高效液相色谱系统已成功应用于三种不同类型水样中氨基多羧酸的测定。流动相的低pH值限制了天然水中金属离子的干扰。当发生这种干扰时,可使用阳离子交换柱来抑制。可测量的最低量为:NTA 75 pg、EDDS 0.7 ng、DTPA 0.8 ng和EDTA 12 ng。该方法还应用于罐装食品中EDTA的测定。