Zhang Jianhua, Cui Huimin, Xu Liangjun, Zhang Lan, Chen Guonan
Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian, P. R. China.
Electrophoresis. 2009 Feb;30(4):674-81. doi: 10.1002/elps.200800569.
This paper describes the use of head-column field-enhanced sample stacking for on-line sample concentration in MEKC; the method has been applied to the determination of C1-C9 aliphatic amines after their pre-capillary derivatization with 3-(4-carboxybenzoyl) quinoline-2-carboxaldehyde (CBQCA). The optimum derivatization, on-line concentration and separation conditions for these aliphatic amines were investigated in detail. The optimized molar ratio of CBQCA to amines was found to be 120:1, and 50 mmol/L borate buffer (pH 9.5) was used for derivatization in order to achieve high efficiency. Nine imidazole aliphatic amines were baseline separated within 12 min by using 50 mmol/L of sodium borate (pH 9.5) and 15 mmol/L of SDS as running buffer. Under the optimum conditions, the detection limits of these nine aliphatic amines ranged from 1.2 to 3.8 pmol/L. S/N=3, which was about 49-173-fold lower than those of conventional sample injections. After validation, the developed method was applied to the determination of C1-C9 aliphatic amines in river water with the average recoveries of 86.7-105%.
本文描述了在毛细管电泳质谱联用（MEKC）中使用柱头场增强进样堆积进行在线样品浓缩；该方法已应用于3-(4-羧基苯甲酰基)喹啉-2-甲醛（CBQCA）对C1-C9脂肪胺进行毛细管前衍生化后的测定。详细研究了这些脂肪胺的最佳衍生化、在线浓缩和分离条件。发现CBQCA与胺的最佳摩尔比为120:1，为了获得高效率，使用50 mmol/L硼酸盐缓冲液（pH 9.5）进行衍生化。通过使用50 mmol/L硼酸钠（pH 9.5）和15 mmol/L十二烷基硫酸钠（SDS）作为运行缓冲液，9种咪唑脂肪胺在12分钟内实现了基线分离。在最佳条件下，这9种脂肪胺的检测限范围为1.2至3.8 pmol/L（信噪比S/N = 3），比传统进样低约49-173倍。经过验证后，所开发的方法应用于河水中C1-C9脂肪胺的测定，平均回收率为86.7-105%。
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