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色谱

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利用瞬间等速电泳的毛细管区带电泳大体积电动进样的研究

李云,何友昭   

  1. Department of Chemistry, University of Science and Technology of China, Hefei 230026, China
  • 收稿日期:2004-02-26 修回日期:1900-01-01 出版日期:2005-01-30 发布日期:1989-03-25
  • 通讯作者: 何友昭
  • 基金资助:

Study on Large-Volume Electrokinetic Injection of Capillary Zone Electrophoresis by Using Transient Isotachophoresis

LI Yun, HE Youzhao   

  1. Department of Chemistry, University of Science and Technology of China, Hefei 230026, China
  • Received:2004-02-26 Revised:1900-01-01 Online:2005-01-30 Published:1989-03-25

PDF

721

被引次数

11

摘要： 采用添加乙腈引发的场放大进样与瞬间等速电泳结合的预富集方法,实现了在毛细管内大体积高盐样品中阳离子的有效富集与分离。详细讨论了影响富集的缓冲体系、尾随离子种类、毛细管有效长度、进样时间和等速电泳时间等重要因素。选择在400 mmol/L LiAc-HAc缓冲液(pH 4.5)和400 mmol/L　β-丙氨酸-HAc尾随液(pH 4.5)及10 kV下样品和尾随溶液电动注入时间分别为270和90 s的条件下对高盐溶液中两种结构相近的药物普萘洛尔和美托洛尔进行了富集和分离。该方法富集倍数约为常规电动进样的280倍，普萘洛尔和美托洛尔的检出限分别为2×10-3和8×10-3 mg/L。

关键词: 场放大进样, 高盐样品 , 毛细管区带电泳, 瞬间等速电泳, 乙腈

Abstract: A sample pre-concentration method that combined field-amplified sample injection (FASI) induced by acetonitrile with transient isotachophoresis was applied to achieve effective concentration and the separation of cations in high-salt samples. Several important factors are discussed, such as buffer systems, terminating ions, column effective length and injection time of sample and terminating solution. A capillary column of 50 μm i.d.×65 cm (effective length of 50 cm) was employed. Solutions of 400 mmol/L LiAc-HAc (pH 4.5) and 400 mmol/L β-alanine-HAc (pH 4.5) were used as buffer solution and terminating electrolyte, respectively. The injection times of sample solution and terminating electrolyte were 270 and 90 s, respectively. Compared with conventional electrokinetic injection, the sensitivity of the proposed method was improved about 280-fold. The detection limits of propranolol and metoprolol achieved 2×10-3 and 8×10-3mg/L, respectively.

Key words: acetonitrile, capillary zone electrophoresis, field-amplified sample injection, high-salt sample , transient isotachophoresis