高效液相色谱法测定双氯芬酸钠凝胶的有关物质  

Determination of Relative Substances in Diclofenac Sodium Gel by HPLC

作　　者：叶汝汉[1,2] 彭蕾 孙晋红 池舒耀 张慧影 张小明 王晓燕 张锻 

机构地区：[1]广州法尔麦兰药物技术有限公司,广东广州510070 [2]中国广州分析测试中心,广东广州510070

出　　处：《分析测试学报》2013年第5期634-638,共5页Journal of Instrumental Analysis

基　　金：广东省科技计划项目(2010A040209001)

摘　　要：建立了双氯芬酸钠凝胶中有关物质的高效液相色谱分离分析方法。采用梯度洗脱的方法对双氯芬酸钠凝胶的有关物质进行分离,流动相A为pH 2.0三氟乙酸溶液-甲醇(80:20),流动相B为乙腈-甲醇(80:20)。采用Waters XBridge色谱柱(5μm,150mm×4.6mm)进行分离,流速为1.0mL/min,进样体积为5μL,二极管阵列检测器,检测波长为254nm,柱温为30℃。在上述色谱条件下,双氯芬酸钠凝胶及特定杂质均在1.0～40.0mg/L质量浓度范围内线性关系良好,相关系数(r)均大于0.99;方法对特定杂质的回收率为97%～104%,相对标准偏差(RSD)不大于3.8%。该法简便、快速、准确、选择性好、灵敏度高,可用于含醇类辅料的双氯芬酸钠凝胶中有关物质的检测。A high-performance liquid chromatographic（HPLC） method was developed for the determination of relative substances in diclofenac sodium gel.The separation of analyte was performed on a Waters XBridge column（5 μm,150 mm×4.6 mm） at a flow rate of 1.0 mL/min and an injection volume of 5 μL,by a gradient elution using pH 2.0 trifluoroacetic acid-methanol（80：20） as mobile phase A and acetonitrile-methanol（80：20） as mobile phase B.The photo-diode array detector（PDA） was set at 254 nm.The column temperature was 30 ℃.Under the above chromatographic conditions,the calibration curves were linear in the range of 1.0-40.0 mg/L with correlation coefficients more than 0.99.The recoveries for all the specified impurities ranged from 97% to 104% with RSDs not more than 3.8%.The proposed method could be applied in the determination of relative substances in diclofenac sodium gel containing alcohols excipients with the advantages of simplicity,rapidity,accuracy,good selectivity and high sensitivity.

关 键 词：双氯芬酸钠凝胶 有关物质 特定杂质 高效液相色谱法 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]