HPLC法测定乙胺吡嗪利福异烟片中有关物质的含量  

Determination of related substances in ethambutol hydrochloride, pyrazinamide, rifampicin and isoniazid tablets by HPLC

作　　者：丁冰 杨文玲 许华容[1] 尹艺迪 毕开顺[1] 李清[1] DING Bing;YANG Wenling;XU Huarong;YIN Yidi;BI Kaishun;LI Qing(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2018年第9期750-755,共6页Journal of Shenyang Pharmaceutical University

基　　金：新药质量评价共性关键技术(2015010201)

摘　　要：目的建立HPLC法测定乙胺吡嗪利福异烟片中已知杂质醌式利福平、N-氧化利福平、3-甲酰利福霉素SV、利福霉素S、利福霉素B、利福霉素SV、吡嗪-2-羧酸、异烟酸和其他未知杂质的含量。方法采用Waters Atlantis T3色谱柱(250 mm×4.60 mm,5μm);流动相A为10 mmol·L^(-1)磷酸氢二钠溶液(用磷酸调节pH至6.8),流动相B为乙腈,梯度洗脱;流速1.0 mL·min^(-1);检测波长254 nm;柱温25℃;进样量20μL。已知杂质采用外标法、未知杂质采用不加校正因子的主成分自身对照法计算含量。结果各待测化合物分离度均良好,供试品中检出杂质含量均低于规定限度。结论所建立的HPLC法能够用于乙胺吡嗪利福异烟片中有关物质的含量测定。Objective To establish an HPLC method for the determination of rifampicin quinone, rifampicin N-oxide, 3-formylrifamycin SV, rifamycin S, rifamycin B, rifamycin SV, 2-pyrazinecarboxylic acid, isonicotinic acid and other unknown impurities in ethambutol hydrochloride, pyrazinamide, rifampicin and isoniazid tablets. Methods The HPLC method was performed on a Waters Atlantis T3 column （250 mmx 4. 60 mm,5 p^m）. Gradient elution was used, and the mobile phase A consisted of 10 mmol ~ L-1 dibasic sodium phosphate buffer （ adjusted to pH of 6. 8 with phosphoric acid） and the mobile phase B was acetonitrile. The flow rate was 1.0 mL 1 min-1. The detection wavelength was set at 254 nm. The column temperature was 25℃. Both the known and unknown impurities were determined by external standard method. Results Impurities could be separated well from rifampin, isoniazid and pyrazinamide and other impurities in tablets. The contents of all impurities were lower than the prescribed limits. Conclusion The established HPLC method is rapid and accurate for the determination of related substances in ethambutol hydrochloride, pyrazinamide, rifampicin and isoniazid tablets.

关 键 词：乙胺吡嗪利福异烟片 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]