Key Laboratory of Eco-chemical Engineering, Ministry of Education, College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao, P. R. China.
Electrophoresis. 2009 Oct;30(19):3449-57. doi: 10.1002/elps.200900020.
A novel method to detect beta-antagonists in rat blood was developed by combining heart-cutting 2-D CE in a single capillary with on-column electrochemical (EC) detection. The blood sample was purified in first dimension by non-micellar CZE separation. Then only a desirable fraction of the first dimension separation was transferred into the second dimension of the capillary by pressure. Finally, the purified sample was separated by MEKC. On-line dual concentration method, field amplified sample stacking and sweeping, was employed to accumulate the purified components that effectively counteracted the sample zone diffusion during the mobilization pressure step. A field decoupler joint and an EC detection cell were employed for on-column EC detection. After optimizing the analytical conditions, the RSD of peak height, peak area and migration time were 2.1-4.3%, 1.5-3.9% and 0.7-1.8% (n=10), respectively. This method has been successfully applied to determine beta-antagonists in postdosing rat blood sample. The pharmacokinetic study also demonstrated that the proposed heart-cutting 2-D CE with on-column EC detection was convenient, sensitive and would become an attractively alternative method for on-line sample cleanup and separation in complex samples.
一种新方法来检测β拮抗剂在大鼠血液中发展了结合心切割二维 CE 在一个单一的毛细管与柱电化学 (EC) 检测。血样在第一维通过非胶束 CZE 分离进行纯化。然后，只有第一维分离的一个理想部分通过压力转移到毛细管的第二维。最后，通过 MEKC 对纯化的样品进行分离。在线双浓度法、场放大样品堆积和扫掠，被用来积累净化的成分，有效地抵消了在加压移动步骤中的样品区扩散。采用场解耦器和 EC 检测池进行柱上 EC 检测。在优化分析条件后，峰高、峰面积和迁移时间的 RSD 分别为 2.1-4.3%、1.5-3.9%和 0.7-1.8%（n=10）。该方法已成功应用于测定给药后大鼠血液中的β拮抗剂。药代动力学研究也表明，所提出的心脏切割二维 CE 与柱上 EC 检测是方便、灵敏的，并将成为一种有吸引力的替代方法，用于在线样品净化和分离复杂样品。
