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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-1poly-β-CD的20mmol.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50mmol.L-1pH 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2.5×10-6~1.25×10-4,5.0×10-7~2.5×10-5,2.5×10-6~1.25×10-4mol.L-1;检出限(S/N=3)分别为5×10-7,1×10-7,5×10-7mol.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: Metoprolol, atenolol and esmolol based on β-adrenergic receptor blocker can obviously enhance the electrochemiluminescence intensity of ternary pyridine ruthenium (Ru (bpy) 32+) A new method for the separation and detection of metoprolol tartrate by capillary electrophoresis and electrochemiluminescence was established. Methods: Poly-β-cyclodextrin (poly-β-CD) was used as separation selection reagent in buffer solution. The optimum conditions for the separation were as follows: 20 mmol.L -1 phosphate solution (pH 10.0) as running buffer solution with a separation voltage of 9 kV and injection voltages of 7.5 kV and 5.5 s respectively. The test cell was a 50 mmol.L-1 pH 8.5 phosphate buffer solution with a working electrode potential of 1.17 V. Results: Atenolol, metoprolol and esmolol were baseline separated within 14 min. The linear range was 2.5 × 10-6 ~ 1.25 × 10-4, 5.0 × 10-7 ~ 2.5 × 10-5 ~ 2.5 × 10-6 ~ 1.25 × 10-4mol.L-1; the detection limits (S / N = 3) were 5 × 10-7, 1 × 10-7 and 5 × 10- 7mol.L-1. The determination of the product of metoprolol betaxolol average content of 24.9 mg. Tablets -1, spiked recoveries between 98.7% to 105%. Conclusion: The method has the characteristics of good separation, high sensitivity, simple and quick. It can be used for the determination of atenolol, metoprolol tartrate and esmolol hydrochloride in the real drug of β-adrenergic receptor blocker.