Department of Chemistry, National Kaohsiung Normal University, Kaohsiung City, Taiwan, ROC.
Department of Chemistry, National Kaohsiung Normal University, Kaohsiung City, Taiwan, ROC.
Talanta. 2015 Jan;131:330-4. doi: 10.1016/j.talanta.2014.08.015. Epub 2014 Aug 13.
High-speed capillary electrophoresis (CE) enables the simple, rapid, and inexpensive analysis of large sets of chiral samples in the pharmaceutical industry. Hence, we developed a novel method for separating enantiomers of d,L-phenothiazines simply and rapidly, based on using poly(diallyldimethylammonium chloride) (PDDAC) as an additive and hydroxypropyl-γ-cyclodextrin (Hp-γ-CD) as a chiral selector in capillary electrophoresis. Adding 0.9% PDDAC to the background electrolyte generated a stable, high, and reversed electroosmotic flow (EOF). Hp-γ-CD not only worked as a complexing agent to increase the chiral resolution between d,L-phenothiazines but also decreased the effective electrophoretic mobility of these drugs. Combining PDDAC and Hp-γ-CD as buffer additives enabled CE to achieve a high-speed enantioseparation of five pairs of d,L-phenothiazines. A decrease in capillary length and an increase in the intensity of the electric field further shortened the separation time. When the background electrolyte contained 0.9% PDDAC, 5mM Hp-γ-CD, and 75 mM formic acid (pH 3.0), enantioseparation of the d,L-phenothiazines was attained within 230 s by applying a capillary length of 32.5 cm and an electric field of 292 V cm(-1). The limit of detection (LOD) of the d,L-phenothiazines at a signal-to-noise ratio of 3 ranged from 2 to 8 μM. We demonstrated the feasibility of this method by detecting the five pairs of d,L-phenothiazines in urine samples.
高速毛细管电泳 (CE) 能够简单、快速且廉价地分析制药行业中大量的手性样品。因此，我们开发了一种新的方法，基于在毛细管电泳中使用聚二烯丙基二甲基氯化铵 (PDDAC) 作为添加剂和羟丙基 -γ-环糊精 (Hp-γ-CD) 作为手性选择剂，简单快速地分离 d,L-吩噻嗪对映体。在背景电解质中添加 0.9% 的 PDDAC 会产生稳定、高且反向的电渗流 (EOF)。Hp-γ-CD 不仅作为络合剂增加了 d,L-吩噻嗪之间的手性分辨率，而且降低了这些药物的有效电泳迁移率。将 PDDAC 和 Hp-γ-CD 结合作为缓冲添加剂，使 CE 能够实现五对对映体 d,L-吩噻嗪的高速对映体分离。缩短毛细管长度和增加电场强度进一步缩短了分离时间。当背景电解质中含有 0.9% 的 PDDAC、5mM 的 Hp-γ-CD 和 75mM 的甲酸 (pH 3.0) 时，通过施加 32.5cm 的毛细管长度和 292Vcm(-1) 的电场，在 230s 内实现了 d,L-吩噻嗪的对映体分离。d,L-吩噻嗪的检测限 (LOD) 在信噪比为 3 时为 2 至 8 μM。我们通过检测尿样中的五对对映体 d,L-吩噻嗪证明了该方法的可行性。
