【摘要】 目的考察利福布丁中微量未知杂质量与其HPLC峰面积的线性关系。方法色谱柱为Hyper-sil-C18(4.6mm×150mm,5μm);流动相为磷酸二氢钾(13.6g/L)—乙腈(50∶50)混合后以2mol/L氢氧化钠调pH为6.5±1,检测波长254nm。配制利福布丁不同浓度梯度的溶液(0.09～2.2mg/ml),并分别进样10μl,读取被考察杂质的峰面积。设0.09mg/ml溶液中被测杂质的量为x0,则其它溶液中该杂质的量分别为2x0～24.44x0。求出该杂质的量(以x0的系数代替)与其色谱峰面积的回归方程的相关系数。结果在杂质浓度约0.36～8.8μg/ml范围内,相关系数为0.9997。结论在上述浓度范围,该杂质的量与其色谱峰面积呈很好的线性关系。同时,相关系数r的数学推导过程表明,r只与x0的系数有关,而与x0无关。因此,这种相关系数的求算方法科学、可靠且简单、直接(无需使用杂质单体),为其他药品中未知杂质的线性关系考察提供了一种新的途径。更多还原

【Abstract】 Objective To investigate the linear relationship between the quantity of unknown minor impurity and its HPLC peak area in rifaputin.Method A Hypersil-C18(4.6mm×150mm,5μm);the mobile phase was a mixture of acetonitrile and 0.1 mol/L monobasic potassium phosphate(50∶50),adjusted by 2mol/L sodium hydroxide to a pH of 6.5±0.1;detected at a wavelength 254nm.A series of rifaputin solutions containing 0.09～2.2mg/ml were prepared and 10μl of the solutions was injected into the chromatograph respectively.The peak area of impurities were recorded.Let x0 equal to the quantity of impurities in 0.09mg/ml solution,then other solutions contain 2x0～24.44x0 of impurities.Calculate the relationship coefficients between the quantity of impurities which were substituted by the coefficient of x0 and the peak area.Results The linear range was 0.36 to 8.8μg/ml;the relationship coefficent was 0.9997.Conclusion The relationship between the quantity of impurities and the peak area was linear;besides,mathematics derivative revealed that relative coefficient was related to x0 coefficient,but not to x0 itself.Therefore,the method of calculating relationship coefficient was scientific,reliable,simple and direct.This method provided a new way for other drugs to investigate linear relationship between unknown impurity and peak area of HPLC.更多还原