Shpak Alexey V, Pirogov Andrey V, Shpigun Oleg A
Chemistry Department, Moscow State University, GSP-2 Vorob'evy Hills, 119992 Moscow, Russia.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Feb 5;800(1-2):91-100. doi: 10.1016/j.jchromb.2003.10.072.
The separation of dansyl (DNS-AAs) and carbobenzoxy (CBZ-AAs) amino acids using micellar electrokinetic chromatography employing polyelectrolyte-surfactant complexes (PSC) formed in the reaction between polyacrylic acid (PAA) and dodecyltrimethylammonium bromide (DTAB) as pseudo-stationary phases was described. The PSCs were stabilized by hydrophobic interactions of alkyl chains of the surfactant ions and converted to an intramolecular micellar-like phase. The running buffer was a 50mM solution of sodium phosphate (pH 6.0) containing 4.6-20.2mM PSC, in which a part of carboxyl groups of PAA was blocked by aliphatic amines. For the systems with 7.9mM of PAA/DTAB complex (phi=0.30, phi-composition of water-soluble polyelectrolyte complex) as a pseudo-stationary phase, the peaks of six dansyl amino acids (DNS-AAs) were baseline resolved. The separation in this case is based on a complex distribution mechanism of the dansyl derivatives between the free buffer and the intramolecular micellar-like phase of the water-soluble PSC. On the other hand, the additives of PAA/DTAB complex (phi=0.30) to the running buffer does not essentially affect on the electrophoretic behaviour of the CBZ-AAs, the variant MEKC is not realized. The influence of the concentration of the complex of PAA/DTAB on the electrophoretic behaviour of analytes was investigated. Relative retentions and relative selectivities were used for describing electrophoretic behaviour of the amino acid derivatives.
描述了使用胶束电动色谱法分离丹磺酰基（DNS - 氨基酸）和苄氧羰基（CBZ - 氨基酸）氨基酸的过程，该方法采用聚丙烯酸（PAA）与十二烷基三甲基溴化铵（DTAB）反应形成的聚电解质 - 表面活性剂复合物（PSC）作为假固定相。PSC通过表面活性剂离子烷基链的疏水相互作用得以稳定，并转变为分子内类似胶束的相。运行缓冲液是含有4.6 - 20.2 mM PSC的50 mM磷酸钠溶液（pH 6.0），其中PAA的一部分羧基被脂肪胺封闭。对于以7.9 mM的PAA/DTAB复合物（φ = 0.30，φ为水溶性聚电解质复合物的组成）作为假固定相的体系，六种丹磺酰基氨基酸（DNS - 氨基酸）的峰实现了基线分离。在这种情况下的分离基于丹磺酰基衍生物在游离缓冲液和水溶性PSC的分子内类似胶束相之间的复杂分配机制。另一方面，向运行缓冲液中添加PAA/DTAB复合物（φ = 0.30）对CBZ - 氨基酸的电泳行为基本没有影响，未实现变体胶束电动色谱。研究了PAA/DTAB复合物浓度对分析物电泳行为的影响。使用相对保留值和相对选择性来描述氨基酸衍生物的电泳行为。
