Optimization of preparative electrophoretic chiral separation of ritalin enantiomers.
Optimization of preparative electrophoretic chiral separation of ritalin enantiomers.
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DOI：
10.1016/s0731-7085(01)00572-6
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发表时间：
2002-01
影响因子：
3.4
通讯作者：
E. Schneiderman;S. R. Gratz;A. Stalcup
中科院分区：
文献类型：
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作者：
E. Schneiderman;S. R. Gratz;A. Stalcup
将连续自由流动电泳(CFFE)应用于利他林对映体的手性拆分。采用硫酸β-环糊精(Sβ-CD)作为手性添加剂。采用液-质联用(LC-MS)法研究了Sβ-CD在分离室中的时间平均浓度。Sβ-CD在分离室中的分布对分离度和偏转角有很大影响。为了优化分离条件，考察了几个参数(甲醇、Sβ-CD在阴极洗涤液和分离缓冲液中的浓度，以及引入低电导区)。利他林对映体的拆分度和偏转角与Sβ-CD在分离缓冲液和阴极洗涤液中的浓度呈非线性关系。在接近最佳条件下，利他林对映体的分离度约为0.8，平均处理速度为0.5 mg/h，单个对映体的纯度为∼83%，而在含有利他林的20个瓶中，只有3个瓶同时检测到这两个对映体。
Continuous free flow electrophoresis (CFFE) was applied to the preparative chiral separation of ritalin enantiomers. Sulfated β-cyclodextrin (sβ-CD) was used as the chiral additive. Liquid chromatography–mass spectrometry (LC–MS) experiments were applied to study the time averaged concentration of sβ-CD in the separation chamber. The distribution of sβ-CD in the separation chamber greatly influenced resolution and the angle of deflection. To optimize the separation, several parameters (methanol, concentration of sβ-CD in the cathodic wash and in the separation buffer, and the introduction of a low conductivity zone) were investigated. The dependence of the resolution and deflection angles of ritalin enantiomers on the concentration of sβ-CD in both the separation buffer and in the cathode wash solution appeared to be non-linear. Under close to optimal conditions, resolution of ritalin enantiomers was about 0.8 with an average processing rate of 0.5 mg/h. Overall, the enantiomeric purity of the individual isomers was ∼83%; however, of the 20 vials containing ritalin, the presence of both enantiomers was only detected in three vials.