Institute of Pharmaceutical Sciences, Department of Pharmaceutical Chemistry, Karl-Franzens-University, Austria.
Electrophoresis. 2009 Aug;30(16):2897-904. doi: 10.1002/elps.200900092.
This work deals with the application of silica-based ligand-exchange chiral stationary phases (CSPs) for the enantioseparation of underivatized amino acids, alpha-hydroxy acids, and dipeptides with packed CEC. Two different possibilities of preparing silica-based CSPs are presented. One phase contains L-4-hydroxyproline chemically bonded via a spacer to 3 mum silica material. The other approach makes use of N-decyl-L-4-hydroxyproline dynamically coated on a reversed-phase packed capillary. Dynamical coating of reversed-phase material represents a simple alternative to prepare CSP. A comparison of the chemically bonded phase with the dynamically coated CSP by means of resolution of complex-forming analytes is presented. The chemically bonded phase was found to be superior to the dynamically coated phase in terms of resolution of amino acids and dipeptides. However, the dynamically coated CSP was found to be especially suitable for the separation of alpha-hydroxy acids. Both techniques are applicable for enantiomer purity tests.
本工作涉及使用基于硅胶的配体交换手性固定相（CSP），通过填充毛细管电色谱（CEC）对手性拆分未衍生的氨基酸、α-羟基酸和二肽进行分析。本文提出了两种制备基于硅胶的 CSP 的不同方法。一种固定相通过间隔臂将 L-4-羟基脯氨酸化学键合到 3 µm 的硅胶材料上。另一种方法则利用 N-癸基-L-4-羟基脯氨酸动态涂覆在反相填充的毛细管上。动态涂覆反相材料是制备 CSP 的一种简单替代方法。通过对形成复合物的分析物的分辨率比较，展示了化学键合相和动态涂覆 CSP 之间的差异。在氨基酸和二肽的分辨率方面，化学键合相优于动态涂覆相。然而，动态涂覆 CSP 特别适用于 α-羟基酸的分离。这两种技术都适用于对映体纯度测试。
