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目的:基于盐酸伊托必利可增强联吡啶钌Ru(bpy)32+的电化学发光的原理,建立运用毛细管电泳-电化学发光法测定盐酸伊托必利。方法:分别优化分离和检测条件,得到最佳分离条件为电极电位1.15 V、进样电压10 kV、进样时间10 s、运行缓冲溶液浓度25 mmol.L-1(pH=8),检测池中的检测条件为5 mmol.L-1的Ru(bpy)23+与50 mmol.L-1的PBS均匀混合。结果:在优化的实验条件下,此法可在200 s内实现盐酸伊托必利的分离和检测,其浓度线性范围为7.0×10-8～1.0×10-5g.mL-1(r=0.9843,n=5),线性方程为I(counts)=1.047×108C+120.8,检出限为5.0×10-9g.mL-1(S/N=3);连续测定5.0×10-6g.mL-1盐酸伊托必利溶液,峰高和迁移时间的RSD分别为3.1%和1.2%(n=7);其平均加样回收率为98.6%～103.7%。结论:本法具有灵敏度高,方便快捷的特点,可用于盐酸伊托必利的药物含量分析。
OBJECTIVE: To establish a method for the determination of itopride hydrochloride by capillary electrophoresis-electrochemiluminescence based on the principle that itoprost hydrochloride can enhance the electrochemical luminescence of Ru (bpy) 32+. Methods: The conditions of separation and detection were optimized respectively. The best separation conditions were as follows: electrode potential 1.15 V, injection voltage 10 kV, injection time 10 s, running buffer concentration 25 mmol.L-1 (pH = 8) The assay conditions were 5 mmol.L-1 of Ru (bpy) 23+ and 50 mmol.L-1 of PBS. Results: Under the optimal experimental conditions, it could be separated and tested in less than 200 s with a linear range of 7.0 × 10-8 ~ 1.0 × 10-5g.mL-1 (r = 0.9843, n = 5), the linear equation was I (counts) = 1.047 × 108C + 120.8 with a detection limit of 5.0 × 10-9g.mL-1 (S / N = 3). The results showed that the RSD of peak height and migration time were 3.1% and 1.2% (n = 7), respectively. The average recoveries of iopride hydrochloride were 98.6% -103.7%. Conclusion: This method has the characteristics of high sensitivity, convenience and quickness, and can be used for the analysis of drug content of Itopride hydrochloride.