Fu Xiaofang, Liu Yi, Li Wei, Pang Nannan, Nie Honggang, Liu Huwei, Cai Zongwei
Beijing National Laboratory for Molecular Sciences, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, Peking University, Beijing, P. R. China.
Electrophoresis. 2009 May;30(10):1783-9. doi: 10.1002/elps.200800487.
A CE-MS method for rapid determination of aristolochic acid-I and aristolochic acid-II (AA-II) in traditional Chinese medicines and biological samples was described in the present paper. AA-I and AA-II can be baseline separated within 6 min by CE-MS with carboxymethyl-chitosan-coated capillary. CZE conditions including pH, concentration of buffer, applied voltage, and capillary temperature were systematically investigated, and the composition and flow rate of sheath liquid were also optimized for CE-MS. Furthermore, the CE-UV method without any additives in BGE solution was established and compared with the CE-MS method. The results showed that the two methods could achieve satisfactory separation efficiency, repeatability, and linearity, while the LOD was 0.6 microg/mL for CE-UV and 0.05 microg/mL for CE-MS. Compared with the CE-UV method, the sensitivity of CE-MS was significantly improved, in addition to the structure information provided by MS detection at the same time. As an application example, a spiked sample in human serum was analyzed by the CE-MS method, indicating that the new CE-MS method can be applied to analyze AAs in biological samples.
本文描述了一种用于快速测定中药和生物样品中马兜铃酸-I和马兜铃酸-II（AA-II）的CE-MS方法。使用羧甲基壳聚糖涂层毛细管的CE-MS可在6分钟内将AA-I和AA-II基线分离。系统研究了CZE条件，包括pH值、缓冲液浓度、施加电压和毛细管温度，还对鞘液的组成和流速进行了CE-MS优化。此外，建立了BGE溶液中无任何添加剂的CE-UV方法，并与CE-MS方法进行了比较。结果表明，两种方法均可实现令人满意的分离效率、重复性和线性，而CE-UV的检测限为0.6μg/mL，CE-MS的检测限为0.05μg/mL。与CE-UV方法相比，CE-MS的灵敏度显著提高，同时还能提供MS检测的结构信息。作为应用实例，采用CE-MS方法分析了人血清中的加标样品，表明新的CE-MS方法可用于分析生物样品中的马兜铃酸。
