Kamande Mary W, Zhu Xiaofeng, Kapnissi-Christodoulou Constantina, Warner Isiah M
Department of Chemistry, Louisiana State University, 434 Choppin Hall, Baton Rouge, Louisiana 70803, USA.
Anal Chem. 2004 Nov 15;76(22):6681-92. doi: 10.1021/ac049313t.
A polyelectrolyte multilayer (PEM) coating consisting of the polypeptide, poly(l-lysine) hydrobromide, poly(l-lysine) and the polymeric dipeptide surfactant, poly(sodium undecanoyl-l-leucyl-alaninate), poly(l-SULA), is investigated as a new medium for the separation of chiral analytes in open-tubular capillary electrochromatography (OT-CEC). In this approach, a stable PEM is constructed in situ by alternative rinses of the cationic polymer poly(l-lysine) and the anionic polymer poly(l-SULA). In previous studies, the PEM coating has been constructed by use of the cationic polyelectrolyte poly (diallydimethylammonium chloride), PDADMAC. In this study, we investigate the use of a biopolymer as the cationic polyelectrolyte. The results reported here indicate an increase in selectivity and resolution when poly(l-lysine) is used as the cationic polymer in place of PDADMAC. To evaluate the chromatographic performance of the PEM coating as a chiral stationary phase, the separation of the beta-blockers, labetalol and sotalol, and the binaphthyl derivatives, 1,1'-bi-2-naphthyl-2,2'-dihydrogen phosphate, 1,1'-bi-2-naphthol, and 1,1-binaphthyl-2,2'-diamine, are investigated. In addition, the effect of varying the amino acid order of the polymeric dipeptide surfactant on resolution is investigated. The number of bilayers also significantly influences the separation efficiency and resolution of enantiomers. The run-to-run and capillary-to-capillary reproducibilities are evaluated by calculating the relative standard deviations (RSDs) of the electroosmotic flow. These RSD values were found to be less than 1%. The coating is also stable and allows more than 290 runs to be performed in the same capillary. In addition, coupling of this chiral OT-CEC column with mass spectrometry is investigated.
一种由多肽、氢溴酸聚（L-赖氨酸）、聚（L-赖氨酸）和聚合二肽表面活性剂聚（十一烷酰-L-亮氨酰丙氨酸钠）（聚（L-SULA））组成的聚电解质多层（PEM）涂层，被研究作为开管毛细管电色谱（OT-CEC）中分离手性分析物的一种新介质。在这种方法中，通过阳离子聚合物聚（L-赖氨酸）和阴离子聚合物聚（L-SULA）的交替冲洗原位构建稳定的PEM。在先前的研究中，PEM涂层是通过使用阳离子聚电解质聚（二烯丙基二甲基氯化铵）（PDADMAC）构建的。在本研究中，我们研究了使用生物聚合物作为阳离子聚电解质的情况。此处报道的结果表明，当使用聚（L-赖氨酸）代替PDADMAC作为阳离子聚合物时，选择性和分辨率有所提高。为了评估PEM涂层作为手性固定相的色谱性能，研究了β-受体阻滞剂拉贝洛尔和索他洛尔以及联萘衍生物1,1'-联-2-萘基-2,2'-二氢磷酸酯、1,1'-联-2-萘酚和1,1-联萘基-2,2'-二胺的分离。此外，还研究了改变聚合二肽表面活性剂的氨基酸顺序对分辨率的影响。双层的数量也显著影响对映体的分离效率和分辨率。通过计算电渗流的相对标准偏差（RSD）来评估批间和毛细管间的重现性。发现这些RSD值小于1%。该涂层也很稳定，允许在同一根毛细管中进行超过290次运行。此外，还研究了这种手性OT-CEC柱与质谱联用的情况。
