He Jun, Shamsi Shahab A
Department of Chemistry, Center of Biotechnology and Drug Design, Georgia State University, Atlanta, GA 30303, USA.
J Chromatogr A. 2009 Jan 30;1216(5):845-56. doi: 10.1016/j.chroma.2008.11.093. Epub 2008 Dec 6.
A mixture of two molecular micelles polysodium N-undecenoxy carbonyl-L-leucinate, (poly-L-SUCL) and polysodium N-undecanoyl leucylvalinate, (poly-L-SULV) was utilized in micellar electrokinetic chromatography-electrospray ionization-mass spectrometry (MEKC-ESI-MS) to simultaneously separate and detect enantiomers of binaphthyl derivatives. Separation parameters such as background buffer composition, voltage, temperature, and nebulizer pressure were optimized using a multivariate central composite design (CCD). Baseline enantioseparation for both analytes was achieved. The CCD was also used in the optimization of sheath liquid and spray chamber parameters to achieve optimum ESI-MS response. The results demonstrate that CCD is a powerful tool for the optimization of MEKC-MS parameters and the response surface model analysis can provide in-depth statistical understandings of the significant factors required to achieve maximum enantioresolution and ESI-MS sensitivity.
将两种分子胶束——N-十一碳烯氧基羰基-L-亮氨酸多钠盐(聚-L-SUCL)和N-十一烷酰亮氨酰缬氨酸多钠盐(聚-L-SULV)的混合物用于胶束电动色谱-电喷雾电离质谱法(MEKC-ESI-MS),以同时分离和检测联萘衍生物的对映体。使用多元中心复合设计(CCD)对背景缓冲液组成、电压、温度和雾化器压力等分离参数进行了优化。两种分析物均实现了基线对映体分离。CCD还用于鞘液和喷雾室参数的优化,以实现最佳的ESI-MS响应。结果表明,CCD是优化MEKC-MS参数的有力工具,响应面模型分析可以提供对实现最大对映体分辨率和ESI-MS灵敏度所需的重要因素的深入统计理解。