Constantinou Andriana S, Nicolaou Irene N, Kapnissi-Christodoulou Constantina P
Department of Chemistry, University of Cyprus, Nicosia, Cyprus.
J Chromatogr Sci. 2012 Mar;50(3):228-36. doi: 10.1093/chromsci/bmr050.
The main objective of this study is the use of polymeric surfactants in polyelectrolyte multilayer (PEM) coatings for the separation of the pharmaceutical substances acetylcholinesterase inhibitors (AChEIs). AChEIs are used for the treatment of Alzheimer's Disease and Myasthenia Gravis. In the open-tubular capillary electrochromatography (OT-CEC) mode, the PEM coating is evaluated using nine AChEIs. Optimal conditions are established by altering several experimental parameters such as the pH of the background electrolyte (BGE), the anionic polymer for the PEM coating, the concentration of NaCl, which is used as an additive in the polymer deposition solutions, the number of bilayers, the deposition time, and the concentration of the polymeric surfactant. 25 mM NaH(2)PO(4).H(2)Ο and 25 mM Na(2)HPO(4) at pH 7 is used as BGE. Two bilayers of poly(diallyl dimethyl ammonium chloride) and poly(sodium N-undecanoyl L-leucinate) provide a baseline separation of all nine analytes in less than 4.5 min. Run-to-run reproducibility studies are also performed, and the relative standard deviation values of the migration times of the nine-analyte peaks are less than 2%. In addition, day-to-day, week-to-week and capillary-to-capillary reproducibilities are evaluated, and the relative standard deviation values of the electroosmotic flow are less than 2%. Finally, using the PEM coating approach, we were able to perform more than 150 runs in the same column. Neither the addition of the polymeric surfactant to the mobile phase, nor the reconstruction of the coating was necessary.
本研究的主要目的是将聚合物表面活性剂用于聚电解质多层（PEM）涂层，以分离药物乙酰胆碱酯酶抑制剂（AChEIs）。AChEIs用于治疗阿尔茨海默病和重症肌无力。在开管毛细管电色谱（OT-CEC）模式下，使用九种AChEIs评估PEM涂层。通过改变几个实验参数来确定最佳条件，如背景电解质（BGE）的pH值、PEM涂层的阴离子聚合物、用作聚合物沉积溶液添加剂的NaCl浓度、双层数、沉积时间和聚合物表面活性剂的浓度。pH值为7的25 mM NaH₂PO₄·H₂O和25 mM Na₂HPO₄用作BGE。聚二烯丙基二甲基氯化铵和聚（N-十一烷酰-L-亮氨酸钠）的两层涂层可在不到4.5分钟内对所有九种分析物进行基线分离。还进行了逐次运行的重现性研究，九个分析物峰迁移时间的相对标准偏差值小于2%。此外，还评估了每日、每周和毛细管间的重现性，电渗流的相对标准偏差值小于2%。最后，使用PEM涂层方法，我们能够在同一根柱子上进行超过150次运行。既无需向流动相中添加聚合物表面活性剂，也无需重新构建涂层。
