Optimization of preparative electrophoretic chiral separation of ritalin enantiomers
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- 作者：Schneiderman ; Eva ; Gratz ; Samuel R. ; Stalcup ; Apryll M.
- 关键词：Ritalin ; Methylphenidate ; Chiral ; Preparative ; Separation ; Continuous free flow electrophoresis ; Capillary electrophoresis ; Deflection angle ; CE ; capillary electrophoresis ; CFFE ; continuous free flow electrophoresis ; β ; -CD ; beta cyclodextrin ; sβ ; -
- 刊名：Journal of Pharmaceutical and Biomedical Analysis
- 出版年：2002
- 出版时间：January 15, 2002
- 年：2002
- 卷：27
- 期：3-4
- 页码：639-650
- 全文大小：995 K
文摘
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.
83 % ; however, of the 20 vials containing ritalin, the presence of both enantiomers was only detected in three vials.