色谱

色谱 ›› 2015, Vol. 33 ›› Issue (9): 988-994.DOI: 10.3724/SP.J.1123.2015.03038

• 研究论文 • 上一篇    下一篇

毛细管电泳-压力辅助电动进样技术对药物西酞普兰的高灵敏检测及手性拆分(英文)

徐中其1,2, 叶峰1, 王永乐1, 李爱梅1   

  1. 1. 东华大学化学化工与生物工程学院, 上海 201620;
    2. 生态纺织教育部重点实验室, 东华大学, 上海 201620
  • 收稿日期:2015-03-27 出版日期:2015-09-08 发布日期:2015-09-09
  • 通讯作者: 徐中其
  • 基金资助:

    Fundamental Research Funds for the Central Universities (15D110533), Ministry of Education of P. R. China.

Pressure-assisted electrokinetic injection stacking for citalopram drug to achieve highly sensitive detection and enantioseparation by capillary electrophoresis

XU Zhongqi1,2, YE Feng1, WANG Yongle1, LI Aimei1   

  1. 1. College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620, China;
    2. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China
  • Received:2015-03-27 Online:2015-09-08 Published:2015-09-09
  • Supported by:

    Fundamental Research Funds for the Central Universities (15D110533), Ministry of Education of P. R. China.

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摘要：

应用压力辅助电动进样(pressure-assisted electrokinetic injection, PAEKI)技术开发了毛细管电泳(CE)对阳离子手性药物西酞普兰(citalopram, CIT)拆分的高灵敏度分析方法。在电动进样(electrokinetic injection, EKI)过程中,由于CIT的两个对映异构体与手性选择试剂(sulfated-β-cyclodextrin, S-β-CD)之间的动态平衡常数存在差异而导致了电动歧视效应。因此,在EKI过程前向毛细管中充满不含手性选择剂的背景电解质,从而抑制电动进样歧视。通过两个步骤优化PAEKI过程中的关键参数得到电渗流和反向压力之间的平衡条件。在最优的PAEKI条件下(+10 kV, 0.2 psi(约1.4 kPa)),两个对映异构体在205 nm紫外检测条件下的检出限(LOD; S/N=3)达到1.1和2.2 ng/mL。灵敏度较常规的压力进样平均提高了62倍,方法的检测灵敏度达到了ng/mL (ppb),有望成为检测人体体液中CIT对映异构体的有效方法。

关键词: 高灵敏度手性拆分, 毛细管电泳, 西酞普兰, 压力辅助电动进样

Abstract:

Pressure-assisted electrokinetic injection (PAEKI) was applied to the highly sensitive enantioseparation of the positively charged drug citalopram (CIT) by capillary electrophoresis (CE). It was found that the injection discrimination occurred in electrokinetic injection (EKI) process due to the different dynamic equilibrium constant between chiral selector (sulfated-β-cyclodextrin, S-β-CD) and two isomers of CIT. Herein, it was proposed to use the background electrolyte (BGE) without chiral selector to fill the capillary, and then start the EKI step to eliminate the injection discrimination of free analytes. The critical parameters in PAEKI could be optimized in two steps to seek the balance between the electroosmotic flow (EOF) and the counterbalance pressure. Under the optimized PAEKI conditions (+10 kV, 0.2 psi (ca. 1.4 kPa)), the obtained LODs (S/N=3) of the two isomers were 1.1 and 2.2 ng/mL under UV detection (205 nm), which was averaged 62-fold improved in comparison with normal hydrodynamic injection (HDI). The proposal offered ng/mL (ppb) level sensitivity of CIT determination and could be an effective method in the applications in human body biofluids.

Key words: capillary electrophoresis (CE), citalopram, highly sensitive enantioseparation, pressure-assisted electrokinetic injection (PAEKI)

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