胶束毛细管电泳同时测定双氯芬酸钠注射液的含量及有关物质  

Simultaneous determination of content and related substances in diclofenac sodium injection by micelle capillary electrophoresis

作　　者：杨直[1] 林丽琴[1] 吴好好[1] 

机构地区：[1]杭州市药品检验所,杭州310017

出　　处：《药物分析杂志》2013年第2期312-316,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：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 micelle capillary electrophoresis method for simultaneous determination of di- elofenae sodium content and 1 - （2,6 - dichlorophenyl） - 1,3 - dihydro - 2H - indol - 2 - one in diclofenac sodi- um injection. Methods ： The analysis was performed on an extended light path （ Bubble Cell） bare fused - silica cap- illary of 75 p.m ×72 cm （ 200 μm of light path） with sodium dodecyl sulfate （SDS） - borate buffer solution （ pH 9.0）. The injection pressure was 5.0 kPa for 3 s, the separation voltage was 30 KV and the wavelength of detection was 242 nm. The column temperature was controlled at 30 ℃. Results： Linear calibration curves were obtained when diclofenac sodium ranged in 0. 1498 mg · mL^-1 -1. 498 mg· mL^-1（ r = 0. 9999, n = 8 ）and 1 - （2,6 -di- chlorophenyl） - 1,3 - dihydro - 2H - indol - 2 - one ranged between 0. 9210 - 9.210 p,g ~ mL - 1 （ r = 0. 9997, n = 8 ） , the LOD of diclofenae sodimn and 1 - （ 2,6 - dichlorophenyl） - 1,3 - dihydro - 2H - indol - 2 - one was 0.25 and 0. 35 μg · mL^-1, respectively. The average recovery was 100. 7% for diclofenac sodium and 99.7% for 1 - （2, 6 - dichlorophenyl） - 1,3 - dihydro - 2H - indol - 2 - one. The repeatability was 0. 81% for diclofenae sodium and 0. 95 % for 1 - （ 2,6 - diehlorophenyl） - 1,3 - dihydro - 2H - indol - 2 - one. Conclusion ： The method is simple, accurate and economic ,which is suitable for the determination of diclofenac sodium and 1 - （2,6 -diehlorophenyl） - 1,3 - dihydro -2H - indol -2 - one in dielofenae sodium injection.

关 键 词：胶束毛细管电泳 双氯芬酸钠 1-(2 6-二氯苯基)-1 3-二氢-2H-吲哚-2-酮 含量测定 有关物质 杂质控制 

分 类 号：R917[医药卫生—药物分析学]