Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan.
J Chromatogr A. 2013 Jun 14;1294:117-21. doi: 10.1016/j.chroma.2013.04.052. Epub 2013 Apr 22.
A tosylated-poly(ethylene oxide) (PEO) reagent was reacted with primary amino groups of an aminopropylsilica packing material (TSKgel NH2-60) in acetonitrile to form PEO-bonded stationary phase. The reaction was a single and simple step reaction. The prepared stationary phase was able to separate inorganic anions. The retention behavior of six common inorganic anions on the prepared stationary phase was examined under various eluent conditions in order to clarify its separation/retention mechanism. The elution order of the tested anions was iodate, bromate, bromide, nitrate, iodide, and thiocyanate, which was similar as observed in common ion chromatography. The retention of inorganic anions could be manipulated by ion exchange interaction which is expected that the eluent cation is coordinated among the PEO chains and it works as the anion-exchange site. Cations and anions of the eluent therefore affected the retention of sample anions. We demonstrated that the retention of the analyte anions decreased with increasing eluent concentration. The repeatability of retention time for the six anions was satisfactory on this column with relative standard deviation values from 1.1 to 4.3% when 10mM sodium chloride was used as the eluent. Compared with the unmodified TSKgel NH2-60, the prepared stationary phase retained inorganic anions more strongly and the selectivity was also improved. The present stationary phase was applied for the determination of inorganic anions contained in various water samples.
将 tosylated-聚(环氧乙烷)(PEO)试剂与氨基丙基硅烷填料(TSKgel NH2-60)的伯氨基在乙腈中反应,形成 PEO 键合固定相。该反应是一个单一且简单的步骤反应。所制备的固定相能够分离无机阴离子。在各种洗脱条件下,考察了六种常见无机阴离子在制备的固定相上的保留行为,以阐明其分离/保留机制。在常规离子色谱中观察到,所测试的阴离子的洗脱顺序为碘酸盐、溴酸盐、溴化物、硝酸盐、碘化物和硫氰酸盐。通过离子交换相互作用可以控制无机阴离子的洗脱,预计洗脱剂阳离子在 PEO 链之间配位,并且作为阴离子交换位点。因此,洗脱剂中的阳离子和阴离子影响样品阴离子的保留。我们证明,随着洗脱剂浓度的增加,分析物阴离子的保留时间减少。当使用 10mM 氯化钠作为洗脱剂时,六种阴离子的保留时间重复性良好,相对标准偏差值在 1.1%至 4.3%之间。与未改性的 TSKgel NH2-60 相比,制备的固定相对无机阴离子的保留更强,选择性也得到了提高。本固定相应用于各种水样中无机阴离子的测定。