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| 毛细管电泳法检测左旋普拉克索中右旋普拉克索杂质的研究 |
| 刘长海1,孙青2,盛春泉2,张海3,陈俊3,赵亮3,柴逸峰1* |
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| (1.第二军医大学药学院药物分析学教研室,上海 200433;2.第二军医大学药学院药物化学教研室,上海 200433;3.第二军医大学东方肝胆外科医院药材科,上海 200438) |
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| 摘要: |
| 目的:建立毛细管电泳法,对左旋普拉克索中右旋普拉克索进行杂质检查。方法:分别以β-环糊精(β-CD)、羟丙基-β-环糊精(HP-β-CD)、硫酸酯-β-环糊精(SBE-β-CD)和二甲基-β-环糊精(DM-β-CD)为手性选择剂,考察手性选择剂的浓度、pH、柱长和柱内径对分离选择性的影响,采用未涂渍熔融石英毛细管47 cm ×50 μm(有效长度40 cm),背景电解质溶液:40 mmol/L柠檬酸三钠缓冲液,含有0.5% SBE-β-CD,用磷酸调节pH值到4.0,柱温:30℃,检测波长254 nm,电压16 kV。 结果:2种旋光异构体的分离度良好(Rs>2.5),样品中右旋普拉克索的含量均小于0.5%。结论:所建立的方法简单可靠、专属性强,可以作为常规的杂质检查手段。 |
| 关键词: 毛细管电泳 手性分离；左旋普拉克索 右旋普拉克索 |
| DOI：10.3724/SP.J.1008.2009.01058 |
| 投稿时间：2008-11-20修订日期：2009-07-31 |
| 基金项目: |
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| Capillary electrophoresis for analysis of optical impurity of L-pramipexole |
| LIU Chang-hai1,SUN Qing-yan2,SHENG Chun-quan2,ZHANG Hai3,CHEN Jun3,ZHAO Liang3,CHAI Yi-feng1* |
| (1.Department of Pharmaceutical Analysis,School of Pharmacy,Second Military Medical University,Shanghai 200433,China;2.Department of Pharmaceutical Chemistry,School of Pharmacy,Second Military Medical University,Shanghai 200433;3.Department of Pharmacy,Eastern Hepatobiliary Hospital,Second Military Medical University,Shanghai 200438) |
| Abstract: |
| Objective:To develop a capillary electrophoresis system for purity test and enantioseparation of L-pramipexole.Methods: Using β-CD,HP-β-CD,SBE-β-CD and DM-β-CD as chiral selection agents,we investigated the influence of concentration,pH of chiral selection agent and column length and inner diameter on chiral separation.The enantiomers were baseline separated under the following conditions-uncoated fused silica capillary (50 μm × 47 cm) with an effective length of 40 cm,back-ground electrolyte solution:40 mmol/l trisodium citrate buffer solution,0.5% SBE-β-CD,pH 4.0 adjusted by phosphoric acid,5% methanol,25 mmol·L-1 SDS,40 mmol·L-1 sodium tetraborate solution as running buffer,and 16 kV separation voltage.The detection wavelength was set at 254 nm and the column temperature was 30℃.Results: The baseline separation of L-pramipexole was obtained under our condition.The optical isomerism had satisfactory resolution (Rs>2.5) and the content of R-pramipexole was less than 0.5%.Conclusion: The proposed method is simple,reliable and can be used for routine purity test and chiral separation. |
| Key words: capillary electrophoresis enantioseparation L-pramipexole R-pramipexole |
