Guo Lei, Matysik Frank-Michael, Gläser Petra, Engewald Werner
Institut für Analytische Chemie, Universität Leipzig, Leipzig, Germany.
Electrophoresis. 2005 Sep;26(17):3341-8. doi: 10.1002/elps.200500188.
The present study is concerned with the application of nonaqueous capillary electrophoresis (NACE) with electrochemical detection (ED) to the separation and quantitative determination of hydrazine (Hy) and its methyl derivatives. The best performance of NACE-ED was found when using 4 mM sodium acetate/10 mM acetic acid/methanol: acetonitrile = 1:2 as the running buffer, with a bare platinum working electrode set at +1.0 V in an end-column amperometric detection cell. The choice and ratio of suitable solvents for the separation and injection media played an essential role for the performance characteristics of the method. The limits of detection for Hy, methylhydrazine, symmetrical dimethylhydrazine, and unsymmetrical dimethylhydrazine were 5, 2, 12, and 1 ng/mL, respectively. This is between one and two orders of magnitude lower than that achieved by previously reported CE-ED methods in aqueous buffer systems in conjunction with various types of chemically modified electrodes. The practical utility of the new NACE-ED methodology is demonstrated in terms of the determination of traces of Hys in spiked environmental samples containing a wide range of explosives and related compounds.
本研究涉及非水毛细管电泳(NACE)结合电化学检测(ED)在肼(Hy)及其甲基衍生物的分离和定量测定中的应用。当使用4 mM醋酸钠/10 mM醋酸/甲醇:乙腈 = 1:2作为运行缓冲液,在柱端安培检测池中使用裸铂工作电极并设置在 +1.0 V时,发现NACE-ED具有最佳性能。合适的分离和进样介质的溶剂选择及比例对该方法的性能特征起着至关重要的作用。Hy、甲基肼、对称二甲基肼和不对称二甲基肼的检测限分别为5、2、12和1 ng/mL。这比先前报道的在水性缓冲体系中结合各种类型化学修饰电极的CE-ED方法所达到的检测限低一到两个数量级。新的NACE-ED方法在含有多种炸药及相关化合物的加标环境样品中痕量Hy的测定方面展示了其实际应用价值。