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目的:建立胶束毛细管电泳法测定双氯芬酸钠注射液的含量以及双氯芬酸杂质A[1-(2,6-二氯苯基)-1,3-二氢-2H-吲哚-2-酮]的含量。方法:采用扩展光程(鼓泡检测池)未涂渍熔融石英毛细管(有效长度:72 cm;内径:75μm;光程:200μm);以十二烷基硫酸钠-硼酸盐缓冲液(pH 9.0)为运行缓冲液;压力进样:5.0 kPa(3 s);操作电压:30kV;检测波长:242nm;毛细管柱温:30℃。结果:双氯芬酸钠和1-(2,6-二氯苯基)-1,3-二氢-2H-吲哚-2-酮分别在0.1498～1.498mg.mL-1(r=0.9999,n=8)和0.9210～9.210μg.mL-1(r=0.9997,n=8)范围内线性关系良好,检测限分别为0.25μg.mL-1和0.35μg.mL-1,准确度分别为100.7%和99.7%,重复性分别为0.81%和0.95%。结论:该方法具有简便、准确、经济的特点,可用于双氯芬酸钠注射液的含量及有关物质测定。
OBJECTIVE: To establish a method for the determination of diclofenac sodium injection by micellar capillary electrophoresis and the determination of diclofenac impurity A [1- (2,6-dichlorophenyl) -1,3-dihydro-2H-indol-2-one] content. Methods: Uncoated fused silica capillaries (effective length: 72 cm; inner diameter: 75 μm; optical path length: 200 μm) were prepared using an extended optical path length (bubbling cell) 9.0) for the running buffer; pressure injection: 5.0 kPa (3 s); operating voltage: 30kV; detection wavelength: 242nm; capillary column temperature: 30 ℃. Results: Diclofenac sodium and 1- (2,6-dichlorophenyl) -1,3-dihydro-2H-indol-2-one were found to be stable at 0.1498-1.498 mg.mL-1 (r = 0.9999, 8) and 0.9210 ~ 9.210μg.mL-1 (r = 0.9997, n = 8). The detection limits were 0.25μg.mL-1 and 0.35μg.mL-1 respectively. The accuracy was 100.7% And 99.7% with repeatability of 0.81% and 0.95% respectively. Conclusion: This method is simple, accurate and economical. It can be used in the determination of diclofenac sodium injection and related substances.