高等学校化学学报 ›› 2012, Vol. 33 ›› Issue (03): 470-474.doi: 10.3969/j.issn.0251-0790.2012.03.007

• 分析化学 • 上一篇    下一篇

非样品手性配体交换毛细管电泳测定手性多巴

邱昌桂1, 王晓瑜1, 郭振朋1, 宋丽娟1, 陈义1,2,3   

  1. 1. 中国科学院化学研究所活体分析化学院重点实验室, 北京 100190;
    2. 北京分子科学国家实验室, 北京 100190;
    3. 北京质谱中心, 北京 100190
  • 收稿日期:2011-04-12 出版日期:2012-03-10 发布日期:2012-03-10
  • 通讯作者: 陈 义, 男, 博士, 研究员, 博士生导师, 主要从事高效高通量生物微分析研究. E-mail:chenyi@iccas.ac.cn
  • 基金资助:

    国家自然科学基金(批准号: 20628507, 20905068), 国家"九七三"计划项目(批准号: 2007CB714504)和中国科学院重要方向项目(批准号: KJCX2-YW-H11)资助.

Chiral Ligand-exchange Capillary Electrophoretic Assay of L-Dopa Tablets Using a Non-analyte Chiral Ligand

QIU Chang-Gui1, WANG Xiao-Yu1, GUO Zhen-Peng1, SONG Li-Juan1, CHEN Yi1,2,3   

  1. 1. Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China;
    2. Beijing National Laboratory for Molecular Science, Beijing 100190, China;
    3. Beijing Center of Mass Spectrometry, Beijing 100190, China
  • Received:2011-04-12 Online:2012-03-10 Published:2012-03-10

摘要:

L-多巴为测定目标, 以天然芳香氨基酸为替代样品, 建立了以非样品α-羟基酸为手性配体, 以铜和镍等二价金属为中心离子的手性配体交换毛细管电泳新方法. 当弱配位的α-羟基酸与中心离子的摩尔比大于6∶1时, 所建立的方法即可实现对D,L-氨基酸和D,L-多巴的基线分离, 可用于口服多巴药片含量的测定, 检测出质量分数为0.5%的异构体杂质, 其定量的线性范围是0.025~2.5 mmol/L, 回收率为96.3%. 据此方法测得某商品药片的实际含量(质量分数)为标称值的(97.33±0.70)%.

关键词: 配体交换毛细管电泳, 羟基酸金属络合物, 手性分离, 氨基酸, 多巴测定

Abstract:

Chiral ligand-exchange capillary electrophoresis is flexible but can not be applied to the analysis of unknown samples or chiral compounds without a chiral ligand. We tried to solve this problem by exploring some non-analyte chiral ligands aiming at the assaying the L-dopa tablets. With aromatic D,L-amino acids (dopa analogues) as mimetic analytes, chiral selecting systems of Cu2+-tartarate and Ni2+-tartarate were obtained among the metal complexes of Cu2+, Ni2+, Zn2+ and Co2+ formed from tartaric, lactic and malic acids. Cu2+-tartarate worked better at an acidic condition while Ni2+-tartarate better at a weakly basic condition. The latter system suited for quantitative analysis of L- and D-dopa in oral tablets. Its linear range was in between 0.025-2.5 mmol/L D- or L-dopa, with linear coefficients all above 0.9999 and recovery at around 96.3%. The detection limit reached about 0.5%(mass fraction) D-dopa. Several batches of L-dopa oral tablets were then assayed, given the content of (97.33?0.70)%(mass fraction) of the specified data. The ratio of ligand to central ion was found to be the most crucial factor, besides, pH and complex concentration were also highly important. Other conditions such as additives and the type of buffer reagents impacted also obviously on the chiral resolution and better optimized.

Key words: Ligand-exchange capillary electrophoresis, Metal-hydroxyl acid complex, Chiral separation, Amino acid, Dopa assay

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