Peterson A G, Ahuja E S, Foley J P
Department of Chemistry, Villanova University, PA 19085-1699, USA.
J Chromatogr B Biomed Appl. 1996 Aug 9;683(1):15-28. doi: 10.1016/0378-4347(96)00188-0.
A novel surfactant with a chiral head group, (R)- or (S)-N-dodecoxycarbonylvaline (DDCV), was used to achieve enantiomeric separations of twenty basic pharmaceutical compounds by micellar electrokinetic chromatography (MEKC). Most of these compounds were beta-agonists (anti-asthmatic, bronchodilators) or beta-antagonists (anti-hypertension, anti-angina). DDCV can separate polar as well as more hydrophobic chiral analytes in the same buffer system. The selectivities for these enantiomeric pairs range from 1.03 to 1.23 with good efficiencies. Separations utilizing DDCV are easy to optimize and allow for exact enantiomeric migration order reversal by switching the enantiomeric form of the surfactant. Buffer systems were assessed to minimize Joule heating and to optimize the repeatability of parameters such as migration time, relative migration time, selectivity, peak areas and area ratios. An electrolyte system consisting of 25 mM DDCV, 100 mM zwitterionic CHES (2-[N-cyclohexylamino]ethanesulfonic acid) and 10 mM triethylamine (TEA) was most effective for these runs. The precision for migration times, relative migration times and selectivities was better than 1%, 0.1% and 1% R.S.D., respectively, while the precision for the area ratios ranged from 1% to 4%. The possible effect of analyte structure on selectivity, efficiency and precision of peak area was studied.
一种具有手性头基的新型表面活性剂，即（R）-或（S）-N-十二烷氧基羰基缬氨酸（DDCV），被用于通过胶束电动色谱法（MEKC）实现20种碱性药物化合物的对映体分离。这些化合物大多是β-激动剂（抗哮喘、支气管扩张剂）或β-拮抗剂（抗高血压、抗心绞痛）。DDCV能够在同一缓冲体系中分离极性以及疏水性更强的手性分析物。这些对映体对的选择性范围为1.03至1.23，分离效率良好。利用DDCV进行的分离易于优化，并且通过切换表面活性剂的对映体形式可以实现对映体迁移顺序的精确反转。对缓冲体系进行了评估，以尽量减少焦耳热，并优化迁移时间、相对迁移时间、选择性、峰面积和面积比等参数的重复性。由25 mM DDCV、100 mM两性离子CHES（2-[N-环己基氨基]乙磺酸）和10 mM三乙胺（TEA）组成的电解质体系对这些实验最为有效。迁移时间、相对迁移时间和选择性的精密度分别优于1%、0.1%和1%（R.S.D.），而面积比的精密度范围为1%至4%。研究了分析物结构对选择性、效率和峰面积精密度的可能影响。
