毛细管电泳-电化学发光法分离和检测酒石酸美托洛尔

目的: 基于β-肾上腺受体阻滞剂药物美托洛尔、阿替洛尔和艾司洛尔均可明显增强三联吡啶络钌(Ru(bpy)₃²⁺)的电化学发光强度的现象,建立了用毛细管电泳-电化学发光法分离和检测酒石酸美托洛尔的新方法。 方法: 以聚合β-环糊精(poly-β-CD)为分离选择试剂添加于缓冲溶液中,通过实验获得优化的分离条件为:含10 mg·mL^-1 poly-β-CD的20 mmol·L^-1的磷酸盐溶液(pH 10.0)为运行缓冲溶液,分离电压9 kV,进样电压和时间分别为7.5 kV和5.5 s。检测池中为50 mmol·L^-1 pH 8.5的磷酸盐缓冲溶液,工作电极电位为1.17 V。 结果: 阿替洛尔,美托洛尔和艾司洛尔3种药物在14 min内实现基线分离;其线性范围分别为2.5×10^-6~1.25×10^-4,5.0×10^-7~2.5×10^-5,2.5×10^-6~1.25×10^-4 mol·L^-1;检出限(S/N=3)分别为5×10^-7,1×10^-7,5×10^-7 mol·L^-1。测定商品药物倍他洛克中美托洛尔平均含量为24.9 mg·片^-1,加标回收率在98.7%~105%之间。 结论: 本方法具有分离效果好,灵敏度高,简便快捷的特点,可用于β-肾上腺受体阻滞剂实际药物中阿替洛尔,酒石酸美托洛尔和盐酸艾司洛尔含量的测定。

Objective: Based on atenolol,metoprolol and esmolol can remarkably enhance tris(2,2'-bipyridyl) ruthenium(Ⅱ)(Ru(bpy)₃²⁺) electrochemiluminescence(ECL) intensity, a novel approach for the separation and determination of metoprolol tartrate was established using capillary electrophoresis coupled with end-column ECL detection. Methods: Parameters affecting separation and detection were optimized by adding poly-β-cyclodextrin(poly-β-CD) into running buffer, respectively, the optimized separation conditions were 20 mmol·L^-1 pH 10.0 phosphate solution containing 10 mg·mL^-1 poly-β-CD as running buffer, a separation potential of 9 kV, a sample injection of 5.0 s at 7 kV. In detection pool, 50 mmol·L^-1 pH 8.5 phosphate was used as running buffer, the potential of work electrode was 1.17 V. Results: Under the optimized experiment conditions, atenolol,metoprolol and esmolol could be baselinely separated and detected within 14 minutes in this method. The ECL intensity were linear with three medicines concentration in the range of 2.5×10^-6-1.25×10^-4,5.0×10^-7-2.5×10^-5 and 2.5×10^-6-1.25×10^-4 mol·L^-1, respectively. And the detection limits(S/N=3) of three medicines were 5×10^-7, 1×10^-7 and 5×10^-7 mol·L^-1, respectively. Conclusion: The developed method is high sensitivity and convenient, which has been successfully applied to detect metoprolol tartrate in betaloc tablets.