HPLC法测定异福酰胺片中有关物质的含量  

Determination of related substances in rifampin,isoniazid and pyrazinamide tablets by HPLC

作　　者：王培香[1] 邢跃文 罗岩[3] 孙艳秀[1] 霍桂兰[1] 孙长山[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]河南煤炭卫生学校,河南平顶山467013 [3]沈阳药大药业有限责任公司,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2013年第2期126-131,共6页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立HPLC法测定异福酰胺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SV、异烟酸、异烟腙和其他未知杂质的含量。方法采用DiamonsilC18(250 mm×4.6mm,5μm)色谱柱,流动相A为磷酸盐缓冲液(10 mmol.L-1磷酸氢二钠溶液,用磷酸调节pH值至6.8)-乙腈(体积比96∶4),流动相B为磷酸盐缓冲液(10 mmol.L-1磷酸氢二钠溶液,用磷酸调节pH值至6.8)-乙腈(体积比55∶45),梯度洗脱,流速为1.0 mL.min-1,检测波长为238 nm,柱温为30℃。已知杂质和未知杂质均采用外标法计算含量。结果各杂质与利福平、异烟肼和吡嗪酰胺分离度良好,样品中醌式利福平、N-氧化利福平、3-甲酰利福霉素SV、利福霉素SV、异烟酸和异烟腙按外标法以峰面积计算其含量分别小于1.5%、1.0%、0.5%、0.5%、1.0%和0.5%,其他未知杂质峰面积的和小于对照溶液中利福平峰面积的3.0%。结论 HPLC法准确、简便、快速,适于测定异福酰胺片中有关物质的含量。Objective To establish an HPLC method for the determination of rifampicin quinone, rifampicin N-oxide ,3-formylrifamycin SV ,rifamycin SV, isonicotinic acid, isoniazone and other unknown impurities in rifampin,isoniazid and pyrazinamide tablets. Methods The HPLC method was performed with the Diamon- sil~ C1~ column（250 mm x4. 6 mm,5 p.m）. The mobile phase A was 10 mmol.L-1 dibasic sodium phos- phate buffer（ adjusted with phosphoric acid to a pH of 6.8 ） and acetonitrile （ V： V = 96： 4） and the mobile phase B was 10 mmol.L-1 dibasic sodium phosphate buffer（ adjusted with phosphoric acid to a pH of 6. 8 ） and acetonitrile（ V： V = 55：45 ）. Gradient elution was used. The flow rate was 1.0 mL. min-l. The detection wavelength was set at 238 nm. The column temperature was 30 ~C. Both the known and unknown impurities were determined by external standard method. Results Impurities could be separated well from rifampin, iso- niazid and pyrazinamide in tablets. The contents of rifampicin quinone ,rifampicin N-oxide ,3-formylrifamy- cin SV, rifamycin SV, isonicotinic acid, isoniazone and other unknown impurities was not more than 1.5 %, 1.0% ,0. 5% ,0. 5% ,1.0% ,0. 5% and 3.0% ,respectively. Contusions The HPLC method is found to be accurate, simple and rapid for the determination of related substances in rifampin, isoniazid and pyrazinamide tablets.

关 键 词：异福酰胺片 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]