非水毛细管电泳法测定双氯芬酸衍生物ZLR-8的含量

Determination of Diclofenac Derivative ZLR-8 by Non-aqueous Capillary Electrophoresis

目的:建立非水毛细管电泳法测定双氯芬酸衍生物ZLR-8[2-(2,6-二氯苯基氨基)苯乙酸-4-(4-苯基-1,2,5-噁二唑-2-氧化物-3-)甲氧基苯甲酯]的含量,探讨甲醇-乙腈比例及醋酸铵浓度对分离选择性及迁移时间的影响.方法:采用未涂层石英毛细管柱(50μm42 cm,有效分离长度为34 cm),以75mmol/L醋酸铵的甲醇-乙腈(30:70)溶液为运行缓冲液,压力5 000 Pa,时间2 s,运行电压为20 kV,柱温20 ℃,检测波长为223 nm.结果:该方法分离效率高,ZLR-8的浓度为0.1～1.0 mg/mL时与峰面积呈良好线性关系(r=0.999 8,n=5),重复性良好(RSD 0.99%,n=6).结论:该方法可作为测定ZLR-8原料药含量的一种方法.

AIM:To develop a non-aqueous capillary electrophoresis method for the assay of NO donating-diclofenac derivative——ZLR-8,and to explore the influence on the electrophoretic behavior of ammonium acetate concentration in the buffer and the ratio of methanol to acetonitrile.METHODS:The separation was performed on an uncoated fused-silica capillary of 50 μm×42 cm,and the running buffer consisted of methanol-acetonitrile (30∶70) containing 75 mmol/L ammonium acetate.Samples were injected by the pressure mode.The applied voltage and the detection wavelength were set at 20 kV and 223 nm,respectively.RESULTS:A good linearity existed over the concentration range of 0.1～1.0 mg/mL(r=0.999 8,n=5),and the RSD for the repeatability was 0.99%(n=6).CONCLUSION:The developed method for the assay of ZLR-8 was simple and rapid.