Mertzman Melissa D, Foley Joe P
Department of Chemistry, Drexel University, Philadelphia, PA 19104, USA.
Electrophoresis. 2004 Feb;25(4-5):723-32. doi: 10.1002/elps.200305736.
In a previous publication (Pascoe, R., Foley, J. P., Analyst 2002, 127, 710-714), a novel chiral microemulsion based on 1.0% w/v dodecoxycarbonylvaline (DDCV), 0.50% v/v ethyl acetate and 1.2% v/v 1-butanol, was shown to provide rapid enantiomeric separations of various pharmaceutical compounds. The two deficiencies noted with this method were that the peak shapes obtained were asymmetric and the efficiencies were lower than those previously obtained using DDCV micelles (Peterson, A. G., Ahuja, E. S., Foley, J. P., J. Chromatogr. B 1996, 683, 15-28). This study examines the use of three alternative low-interfacial-tension oils (methyl acetate, methyl propionate, and methyl formate), in combination with DDCV, to characterize their effect on the elution range, efficiency, resolution, and enantioselectivity of various pharmaceutical enantiomers. The oils were evaluated in both the same volume percentage and the same molar concentration as ethyl acetate in the original DDCV microemulsion system. Including ethyl acetate, a total of seven microemulsion systems were examined. For the compounds that were separated, average enantioselectivities ranged from 1.09 to 1.28, with corresponding efficiencies of 14,000-20,000. While some interesting differences were observed, ethyl acetate still proved to be the most advantageous in terms of enantioselectivity, resolution, and elution range.
在之前的一篇文献(帕斯科,R.,福利,J.P.,《分析家》2002年,127卷,710 - 714页)中,一种基于1.0%(w/v)十二烷氧基羰基缬氨酸(DDCV)、0.50%(v/v)乙酸乙酯和1.2%(v/v)正丁醇的新型手性微乳液,被证明能快速实现多种药物化合物的对映体分离。该方法存在的两个不足之处在于,得到的峰形不对称,且效率低于之前使用DDCV胶束时获得的效率(彼得森,A.G.,阿胡贾,E.S.,福利,J.P.,《色谱杂志B》1996年,683卷,15 - 28页)。本研究考察了三种替代的低界面张力油(乙酸甲酯、丙酸甲酯和甲酸甲酯)与DDCV结合使用时,对各种药物对映体的洗脱范围、效率、分离度和对映选择性的影响。这些油在与原始DDCV微乳液体系中乙酸乙酯相同的体积百分比和相同的摩尔浓度下进行评估。包括乙酸乙酯在内,总共考察了七种微乳液体系。对于被分离的化合物,平均对映选择性范围为1.09至1.28,相应效率为14,000 - 20,000。虽然观察到了一些有趣的差异,但就对映选择性、分离度和洗脱范围而言,乙酸乙酯仍然被证明是最具优势的。