Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources, Ministry of Education of China, College of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin, China.
J Chromatogr A. 2010 Jul 9;1217(28):4753-6. doi: 10.1016/j.chroma.2010.05.021.
A simple, sensitive and selective determination of diltiazem hydrochloride (DLT) is described using capillary electrophoresis electrochemiluminescence (CE-ECL). The CE-ECL parameters that affect separation and detection were optimized. Under the optimized conditions, the linear range of DLT was from 0.02 to 100 μmol/L (r(2) = 0.9983), with the detection limit of 5.1 nmol/L (3σ). The relative standard deviations of ECL intensity and the migration time were <2% for 0.1 μmol/L and 22 μmol/L DLT (n = 11). A new technique for determining of the number of binding sites and binding constant between DLT and HSA was developed using ultrasonic microdialysis coupled with CE-ECL. The number of binding sites and binding constant were 5.9 and 6.3 × 10(4) L/mol, respectively. The time required for ultrasonic microdialysis was 10 times less than that for traditional dialysis. Compared with traditional dialysis, ultrasonic microdialysis is simple, rapid, and should be applicable to a wide range of interactions of drugs and biomacromolecules.
采用毛细管电泳电化学发光(CE-ECL)法,描述了一种简单、灵敏、选择性测定盐酸地尔硫卓(DLT)的方法。优化了影响分离和检测的 CE-ECL 参数。在优化条件下,DLT 的线性范围为 0.02-100 μmol/L(r(2) = 0.9983),检测限为 5.1 nmol/L(3σ)。对于 0.1 μmol/L 和 22 μmol/L 的 DLT(n = 11),ECL 强度和迁移时间的相对标准偏差均<2%。采用超声微透析与 CE-ECL 联用,建立了一种测定 DLT 与 HSA 之间结合位点数和结合常数的新方法。结合位点数和结合常数分别为 5.9 和 6.3×10(4) L/mol。超声微透析所需时间比传统透析少 10 倍。与传统透析相比,超声微透析简单、快速,应适用于广泛的药物与生物大分子相互作用。