Department of Analytical Pharmaceutical Chemistry, Institute of Pharmacy, University of Liège, Liège, Belgium.
Electrophoresis. 2009 Aug;30(16):2862-8. doi: 10.1002/elps.200800824.
The separation of ten beta-blockers has been investigated in NACE systems using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-CD (HDMS-beta-CD) and heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-CD (HDAS-beta-CD). The influence on enantioresolution, mobility difference and selectivity of the nature of both anionic CD and BGE anion as well as their concentrations were studied by means of a multivariate approach. A D-optimal design with 25 experimental points was applied. For all studied analytes, the enantiomeric resolution was shown to be significantly influenced by both CD nature and concentration. Except for two compounds, HDAS-beta-CD was found to give higher enantioresolution values than HDMS-beta-CD. The best enantioseparation for all compounds was achieved in the presence of a high chiral selector concentration and for most of them at a low BGE anion concentration. For each investigated compound, operating conditions leading to the best enantiomeric resolution were deduced. A generic NACE system was then recommended, namely 10 mM ammonium acetate and 40 mM HDAS-beta-CD in methanol acidified with 0.75 M formic acid. This generic system was able to completely resolve the enantiomers of all beta-blockers, with a R(s) value of at least 4. Finally, the optimal conditions obtained modelling resolution, mobility difference and selectivity were compared.
已在 NACE 体系中用七（2,3-二-O-甲基-6-O-磺酸基）-β-CD（HDMS-β-CD）和七（2,3-二-O-乙酰基-6-O-磺酸基）-β-CD（HDAS-β-CD）研究了 10 种β-阻滞剂的分离。通过多元方法研究了阴离子 CD 和 BGE 阴离子的性质及其浓度对映体拆分度、迁移率差异和选择性的影响。应用了具有 25 个实验点的 D-最优设计。对于所有研究的分析物，对映体拆分度均明显受到 CD 性质和浓度的影响。除了两种化合物外，HDAS-β-CD 被发现比 HDMS-β-CD 具有更高的对映体拆分度。对于所有化合物，在高手性选择器浓度下，并且对于大多数化合物在低 BGE 阴离子浓度下，均实现了最佳的对映体分离。为每种研究的化合物推导出了获得最佳对映体分辨率的操作条件。然后推荐了一个通用的 NACE 系统，即 10 mM 乙酸铵和 40 mM 甲醇中酸化的 HDAS-β-CD，其中甲酸浓度为 0.75 M。该通用系统能够完全拆分所有β-阻滞剂的对映异构体，R(s)值至少为 4。最后，比较了模型分辨率、迁移率差异和选择性的最佳条件。
