Mangelings Debby, Discry Jérôme, Maftouh Mohamed, Massart D Luc, Vander Heyden Yvan
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
Electrophoresis. 2005 Oct;26(20):3930-41. doi: 10.1002/elps.200500079.
In completion of an earlier defined generic chiral screening approach, a generic separation strategy for basic, bifunctional, and neutral compounds was proposed and evaluated. This strategy adds to a previously defined strategy for acidic compounds. The screening experiment of the actual strategy used a mobile phase of 5 mM phosphate buffer pH 11.5/ACN (30/70 v/v), a temperature of 25 degrees C, and a voltage of 15 kV. The selected chiral stationary phases were Chiralpak AD-RH, Chiralcel OD-RH, Chiralcel OJ-RH, and Chiralpak AS-RH, all based on polysaccharide selectors. It was seen that 31 out of 48 test compounds were partially or baseline-resolved under screening conditions. After execution of the optimization steps of the strategy, this number increased to 41, with a total of 21 baseline-separated compounds. Combined with the results obtained from the acidic test set examined in the earlier defined strategy, of all tested compounds 82.5% showed enantioselectivity and 49.2% could be baseline-separated.
在完成早期定义的通用手性筛选方法后，提出并评估了一种针对碱性、双官能团和中性化合物的通用分离策略。该策略补充了先前针对酸性化合物定义的策略。实际策略的筛选实验使用了pH 11.5的5 mM磷酸盐缓冲液/乙腈（30/70 v/v）的流动相、25℃的温度和15 kV的电压。所选的手性固定相为Chiralpak AD-RH、Chiralcel OD-RH、Chiralcel OJ-RH和Chiralpak AS-RH，均基于多糖选择剂。可以看出，48种测试化合物中有31种在筛选条件下实现了部分或基线分离。在执行该策略的优化步骤后，这一数字增加到41，共有21种化合物实现了基线分离。结合早期定义策略中酸性测试集的结果，所有测试化合物中82.5%表现出对映选择性，49.2%可以实现基线分离。
