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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DiamonsilC18(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 a HPLC method for determination of rifampicin, rifampin N-oxide, rifavirin SV, isonicotinic acid, isoniazid and Other unknown impurity content. Methods Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase A was phosphate buffer (10 mmol·L -1 disodium hydrogen phosphate solution, adjusted to pH 6.8 with phosphoric acid) 96: 4). The mobile phase B was a phosphate buffer solution (10 mmol·L -1 disodium hydrogen phosphate solution, adjusted to pH 6.8 with phosphoric acid) -acetonitrile (55:45 by volume) 1.0 mL.min-1, the detection wavelength was 238 nm, the column temperature was 30 ℃. Known impurities and unknown impurities are calculated using the external standard content. Results The impurities were separated well from rifampin, isoniazid and pyrazinamide. The samples were rifampin quinone, rifampicin N-oxide, SV, rifamycin SV, Isonicotinic acid and isonicotinic hydrazone were less than 1.5%, 1.0%, 0.5%, 0.5%, 1.0% and 0.5% respectively according to the peak area by external standard method. The sum of peak areas of other unknown impurities was less than that of the control solution Flat peak area of 3.0%. Conclusion HPLC method is accurate, simple and rapid and suitable for the determination of related substances in isoformic acid tablets.