乙胺吡嗪利福异烟片中各组分的高效液相测定方法  

HPLC determination of active components in Yi'an Biqin Lifu Yiyan tablets

作　　者：郭涛[1] 颜鸣[1] 宋洪涛[1] 何仲贵[2] 刘明妍[1] 储晓琴[1] 李妍妍[3] 

机构地区：[1]沈阳军区总医院药剂科,沈阳110016 [2]沈阳药科大学,沈阳110016 [3]沈阳红旗制药有限公司,沈阳110026

出　　处：《药物分析杂志》2007年第4期528-531,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立高效液相色谱法测定乙胺吡嗪利福异烟片中盐酸乙胺丁醇、吡嗪酰胺、利福平和异烟肼含量。方法:盐酸乙胺丁醇选用了苯乙基异氰酸酯为衍生剂进行柱前衍生化,用C_(18)色谱柱,甲醇-水-冰醋酸(70∶30∶0.2)为流动相,流速1.0mL·min^(-1),检测波长220nm。异烟肼和吡嗪酰胺用C_(18)色谱柱,以乙腈-0.02mol·L^(-1)磷酸二氢铵(2∶98)为流动相,流速1.0mL·min^(-1),检测波长263nm。利福平色谱条件为C_(18)色谱柱,以甲醇-乙腈-0.075mol·L^(-1)磷酸二氢钾-1mol·L^(-1)枸橼酸(30∶30∶26∶4)为流动相,流速1.0mL·min^(-1),检测波长254nm。结果:盐酸乙胺丁醇、异烟肼、吡嗪酰胺及利福平分别在20～160,2～50,10～250,20～180μg·mL^(-1)的浓度范围内,呈良好的线性关系。结论:各成分测定方法简便,重现性好,特别是盐酸乙胺丁醇的衍生化方法反应迅速,条件容易控制,衍生化方法可靠,适用于抗结核固定剂量复合剂多成分的分离和含量测定。Objective：To set up the method for the determination of ethambutol hydrochloride isoniazid, pyrazinamide, and rifampicin in Yi＇an Biqin Lifu Yiyan tablets by HPLC. Method：Ethambutol hydrochloride with phenylethyl isocyanate by precolumn derivation were detected with C ls column, the mobile phase was methanol -water- glacial acetic acid （70： 30： 0. 2） and the flowing rate was 1.0 mL · min^-1 ,detected at 220 nm. Isoniazid and pyrazinamide in the tablets were separated on the column of C18, and the mobile phase consisted of acetonitrile -0. 02 mol · L^-1 ammonium dihydrogen phosphate （2： 98）. The flowing rate was 1.0 mL · min^-1 with UV detection at 263 nm. The chromatographic conditions of rifampicin were as follows： C18 column,with a mixture the mobile phase of methanol -acetonitrile- 0. 075 mol ·L^- 1 potassium dihydrogen phosphate -1 mol ·L^- 1 citric acid （30： 30：26： 4）, a flowing rate of 1.0 mL ·min^- 1, and the detective wavelength at 254 nm. Result：The linear ranges of ethambutol hydrochloride, isoniazid, pyrazinamide, and rifampicin were 20 - 160,2 - 50,10 - 250,20 - 180 μg·mL^-1, respectively. Conclusion：The determination method of different components appeared to be simple with a good reproducibility. Especially the derivating reaction of ethambutol hydrochloride,was rapid, reliable and controlled easily. The method can be used for the content determination of ethambutol hydrochloride in fixed - dose combination （FDC）.

关 键 词：乙胺吡嗪利福异烟片 固定剂量复合剂 异烟肼 吡嗪酰胺 盐酸乙胺丁醇 利福平 

分 类 号：R917[医药卫生—药物分析学]