Stern E, Goossens L, Vaccher C, Bonte J-P, Depreux P, Henichart J-P, Goossens J-F
Institut de Chimie Pharmaceutique Albert Lespagnol, EA 2692, Université de LILLE 2-BP 83, 3 rue du Pr. Laguesse, 59006 Lille, France.
J Pharm Biomed Anal. 2008 Apr 14;46(5):848-53. doi: 10.1016/j.jpba.2007.01.044. Epub 2007 Feb 3.
Analytical HPLC methods using derivatized amylose chiral stationary phases, Chiralpak AD-H and Chiralpak AS, were developed for the direct enantioseparation of eight substituted 4-oxo-1,4-dihydroquinoline-3-carboxamide derivatives with one stereogenic center. Baseline separation (Rs>1.5) was always achieved on amylose based Chiralpak AD-H column to the difference with Chiralpak AS. Using UV detection, a linear response was observed within a 180-420 micromol L(-1) concentration range (r2>0.991) for three racemic compounds 1, 3 and 4 with best pharmacological potentials; repeatability, limit of detection (LD) and quantification (LQ) were also determined: LD varied, for the solutes, from 0.36 to 2.56 micromol L(-1). Finally, the enantiopurity of these compounds was determined. Additionally, the effect of temperature variations upon isomer separations was investigated.
采用衍生化直链淀粉手性固定相Chiralpak AD - H和Chiralpak AS的高效液相色谱分析方法，用于直接对映体分离8种具有一个手性中心的取代4 - 氧代 - 1,4 - 二氢喹啉 - 3 - 甲酰胺衍生物。与Chiralpak AS不同，在基于直链淀粉的Chiralpak AD - H柱上总能实现基线分离（Rs>1.5）。使用紫外检测，对于三种具有最佳药理潜力的外消旋化合物1、3和4，在180 - 420 μmol L(-1)浓度范围内观察到线性响应（r2>0.991）；还测定了重复性、检测限（LD）和定量限（LQ）：溶质的LD在0.36至2.56 μmol L(-1)之间变化。最后，测定了这些化合物的对映体纯度。此外，研究了温度变化对异构体分离的影响。
