滴眼用利福平原料中有关杂质的检测  

Determination of Related Impurities in Rifampicin for Eye Use by HPLC

作　　者：胡泽锴 张洁 熊雯 HU Ze-kai;XIONG Wen(Chengdu Institute for Food and Drug control, Chengdu 610045, China)

机构地区：[1]成都市食品药品检验研究院,成都610045

出　　处：《抗感染药学》2018年第5期750-752,共3页Anti-infection Pharmacy

摘　　要：目的:建立滴眼用利福平原料中有关杂质(醌式利福平、3-甲酰利福霉素SV、N-氧化利福平)的高效液相色谱法(HPLC)检测方法。方法:以辛基硅烷键合硅胶为填充剂,采用乙腈-甲醇-磷酸二氢钾溶液(0.075 mol/L)-柠檬酸溶液(1.0 mol/L)(30∶30∶36∶4)为流动相,在波长254 nm处检测,检测流速为1.0 m L/min,分析原料中3种杂质的含量。结果:利福平及3种杂质的对照品在各自的浓度范围内呈现良好的线性关系(r^2=0.999 6~0.999 9,n=5),最低检出限范围介于0.1~0.3μg/m L。结论:该方法的检测灵敏度、精密度和准确度较高,线性关系良好,能够满足对滴眼用利福平原料质量的控制要求。Objective： To establish the determination by a high performance liquid chromatography（HPLC） for detecting impurities（quinoid rifampicin, 3-methyrifamycin SV and N-rifampicin） in rifampicin raw materials. Methods： Using octyl silicane bonded silica gel as filler; and acetonitrile-methanol-dihydrogen phosphate solution（0.075 mol/L）-citric acid solution（1.0 mol/L）（30：30：36：4） were used for mobile phase. At wavelength 254 nm, the flow rate was 1.0 m L/min. The contents of three impurities in raw materials were analyzed. Results： Linear relationships were obtained for the rifampicin and 3 kinds of impurities in concentration ranges respective, correlation coefficient were between r^2=0.999 6 and 0.999 9（n=5）, and the minimum detectable range was between 0.1 μg/m L and 0.3 μg/m L. Conclusion： The method showed the advantages of high sensitivity, good accurancy and linearity, which could be used for the determination of residual solvents in related substances in rifampicin for eye use.

关 键 词：滴眼用利福平 有关杂质 醌式利福平 3-甲酰利福霉素SV N-氧化利福平 残留溶剂 HPLC 

分 类 号：R927[医药卫生—药学]