Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research (CePhaR), Vrije Universiteit Brussel-VUB, Laarbeeklaan 103, B-1090 Brussels, Belgium.
J Pharm Biomed Anal. 2011 Jun 1;55(3):414-23. doi: 10.1016/j.jpba.2011.02.015. Epub 2011 Feb 17.
Four recently commercialized polysaccharide-based chiral stationary phases, Sepapak(®) 1, Sepapak(®) 2, Sepapak(®) 3, and Sepapak(®) 4, now called Lux(®) Cellulose-1, Lux(®) Cellulose-2, Lux(®) Amylose-2 and Lux(®) Cellulose-4, respectively, were examined for their enantioselectivity on a set of 61 racemic compounds by applying the screening conditions of a previously developed chiral screening strategy in normal phase liquid chromatography (NPLC) [N. Matthijs et al., J. Chromatogr. A 1041 (2004) 119-133]. The enantioselectivity on these phases was compared to that on the initial set of polysaccharide-based phases, Chiralpak(®) AD-H, Chiralcel(®) OD-H, and Chiralcel(®) OJ-H, used in the earlier defined strategy. The results showed that 53 compounds out of 61 (86.9%) were resolved on the initial set of chiral stationary phases (CSPs) using two mobile phases per compound, either heptane-ethanol-diethylamine (DEA) or heptane-isopropanol-DEA for testing basic compounds and heptane-ethanol-trifluoroacetic acid (TFA) or heptane-isopropanol-TFA for acidic, bifunctional and neutral compounds. The recently commercialized set of columns gave 54 separations in total (88.5%). Our results indicated that ethanol (EtOH) as polar modifier provides a higher success rate and better resolutions than isopropanol (IPA) on both sets of stationary phases. However, the usefulness of the mobile phase with IPA as polar modifier cannot be neglected for complementarity reasons. It was found that the screening is improved by the introduction of the recently commercialized polysaccharides based CSPs since they provided enantioseparation for compounds that were not resolved by the traditional CSPs. The combination between the initial and the recently commercialized CSPs showed enantioresolution for 55 compounds out of 61 (90%), among which 47 were baseline resolved.
四种最近商业化的多糖手性固定相，Sepapak(®) 1、Sepapak(®) 2、Sepapak(®) 3 和 Sepapak(®) 4，现在分别称为 Lux(®) Cellulose-1、Lux(®) Cellulose-2、Lux(®) Amylose-2 和 Lux(®) Cellulose-4，通过应用先前开发的正相液相色谱 (NPLC) 手性筛选策略的筛选条件，对 61 种外消旋化合物进行了对映选择性研究 [N. Matthijs 等人，J. Chromatogr. A 1041 (2004) 119-133]。这些固定相的对映选择性与先前定义的策略中使用的最初的多糖手性固定相 Chiralpak(®) AD-H、Chiralcel(®) OD-H 和 Chiralcel(®) OJ-H 进行了比较。结果表明，在最初的一组手性固定相（CSP）上，使用两种移动相（每化合物一种），分别为庚烷-乙醇-二乙胺（DEA）或庚烷-异丙醇-DEA 测试碱性化合物和庚烷-乙醇-三氟乙酸（TFA）或庚烷-异丙醇-TFA 测试酸性、多功能和中性化合物，61 种化合物中的 53 种（86.9%）得到拆分。最近商业化的一组柱子总共给出了 54 种分离（88.5%）。我们的结果表明，乙醇（EtOH）作为极性改性剂在手性固定相上提供了比异丙醇（IPA）更高的成功率和更好的分辨率。然而，由于互补性原因，IPA 作为极性改性剂的移动相的用途不可忽视。结果发现，通过引入最近商业化的多糖基 CSP，筛选得到了改善，因为它们为传统 CSP 未拆分的化合物提供了对映体分离。最初和最近商业化的 CSP 的组合显示出对 61 种化合物中的 55 种（90%）的对映体分辨率，其中 47 种是基线分离的。
