改进HPLC法测定吲哚美辛肠溶片中的有关物质.PDFVIP

改进HPLC 法测定吲哚美辛肠溶片中的有关物质 ＊ 李 超 （重庆市食品药品检验检测研究院，重庆 401121） 中图分类号 R927.2 文献标志码 A 文章编号 1001-0408（2016）27-3861-04 DOI 10.6039/j.issn. 1001-0408.2016.27.39 摘 要 目的：改进高效液相色谱法测定吲哚美辛肠溶片中2- 甲基-5- 甲氧基-1H-吲哚-3-乙酸（以下简称杂质Ⅰ）和4-氯苯甲酸 （以下简称杂质Ⅱ）的含量。方法：色谱柱为Phenomenex Phenyl-Hexyl ，流动相为10g/L 醋酸溶液- 乙腈（梯度洗脱），流速为 1.0ml/min ，检测波长为254nm ，柱温为40 ℃，进样量为20μl。结果：杂质Ⅰ和杂质Ⅱ的检测质量浓度线性范围分别为0.2622～ 5.2430、0.2525～5.0500μg/ml（r 均为0.9998）；定量限分别为1.12、0.48ng ，检测限分别为0.340、0.146ng ；精密度、稳定性、重复性 试验的RSD ＜2％；杂质Ⅰ和杂质Ⅱ的加样回收率分别为99.71％～100.52％（RSD ＝0.28％，n ＝9）、100.84％～102.14％（RSD ＝ 0.47％，n ＝9）。结论：该方法准确、快速，可用于吲哚美辛肠溶片中杂质Ⅰ和杂质Ⅱ的含量测定。 关键词 高效液相色谱法；吲哚美辛肠溶片；2- 甲基-5- 甲氧基-1H-吲哚-3-乙酸；4-氯苯甲酸 Determination of Related Substance in Indometacin Enteric-coated Tablet by Improving HPLC LI Chao （Chongqing Institute For Food and Drug Control ，Chongqing 401121，China ） ABSTRACT OBJECTIVE ：To improve HPLC for the contents determination of 2-methyl-5-methoxy-indole-3-acetic acid （impuri- ty Ⅰ）and 4-chlorobenzoic （impurity Ⅱ）in Indometacin enteric-coated tablet. METHODS ：The column was Phenomenex Phe- nyl-Hexyl with mobile phase of 10g/L acetic acid solution - acetonitrile （gradient elution ）at a flow rate of 1.0 ml/min ，the detec- tion wavelength was 254 nm ，column temperature was 40℃，injection volume was 20 μl. RESULTS ：The linear range was 0.262 2-5.243 0 μg/ml for impurity Ⅰ（r ＝0.999 8）and 0.252 5-5.050 0 μg/ml for impurity Ⅱ（r ＝0.999 8）；the limits of quanti- tation were 1.12ng and 0.48ng ，limits of detection were 0.340ng and 0.146ng ，respectively ；RSDs of precision ，stability and re- producibility tests were lower than 2％；recoveries were 99.71％-100.52％（RSD＝0.28％，n＝9）and 100.84％-102.14％（RSD ＝ 0.47％，n ＝9）. CONCLUSIONS ：The method is accurate and rapid ，and can be used for the contents determination of impurity Ⅰ and impurity Ⅱin Indometacin enteric-coated tablet. KEYWORDS HPLC ；Indometacin enteric-coated tablet ；2-methyl-5-met