Cluster of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima, 960-1296, Japan; Institute of Environmental Radioactivity, Fukushima University, 1 Kanayagawa, Fukushima, 960-1296, Japan.
Cluster of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima, 960-1296, Japan.
J Chromatogr A. 2020 Jun 21;1621:461033. doi: 10.1016/j.chroma.2020.461033. Epub 2020 Mar 11.
A diethylammonio-propylsulfate amphoteric ionic resin was synthesized and employed as the stationary phase for high-performance liquid chromatography-mass spectrometry (LC-MS) separation and detection of amino acids. The influence of experimental conditions such as mobile phase composition, column length and temperature upon the amino acid separations was evaluated. However, temperature, addition of water-miscible organic solvent to the mobile phase and mobile phase gradients were not effective at improving the separations. In contrast, the use of an unbuffered pure water mobile phase proved successful for the separation and detection of amino acids. The observed order of elution seems to parallel the isoelectric points of the respective amino acids and suggests that this diethylammonio-propylsulfate stationary phase column functions as an amphoteric ion-exchanger. Under optimized chromatographic conditions, the detection limits for the amino acids were in range of 0.07-0.44 pmol (pico-mole). The method was also successfully applied for the analysis of an actual commercial sample.
一种二乙氨丙基硫酸酯两性离子树脂被合成并用作高效液相色谱-质谱（LC-MS）分离和检测氨基酸的固定相。考察了实验条件如流动相组成、柱长和温度对氨基酸分离的影响。然而，温度、向流动相中添加与水混溶的有机溶剂以及流动相梯度对改善分离效果并不有效。相比之下，使用无缓冲的纯水流动相成功地实现了氨基酸的分离和检测。观察到的洗脱顺序似乎与各氨基酸的等电点平行，表明这种二乙氨丙基硫酸酯固定相柱作为两性离子交换剂起作用。在优化的色谱条件下，氨基酸的检测限在 0.07-0.44 pmol（皮摩尔）范围内。该方法还成功地应用于实际商业样品的分析。
