【摘要】 为测定马西替坦片中的有关物质,利用高效液相色谱法,用十八烷基硅烷键合硅胶为填充剂,以水(1 000 m L水,加入三乙胺1 m L,用磷酸调至p H值=3.0)为流动相A,乙腈为流动相B,梯度洗脱,检测波长为220 nm,柱温40℃,流速1.0 m L/min,进样量10μL.实验显示,在各破坏条件下产生的杂质与主峰以及杂质与杂质之间分离度均在1.5以上,能达到完全分离,杂质MAA6-1、MAA6-2、MAA7-3、MAA6检测限分别为0.019ng、0.013 ng、0.072 ng、0.108 ng,峰面积与浓度呈良好的线性关系,校正因子都为1.0.结果表明,本方法简单、准确度高,专属性强,适用于马西替坦片中有关物质的测定.更多还原

【Abstract】 The paper establishes an HPLC method for the determination of the related substances in macitentan. The silane bonded silica is used as filler,with water( 1 000 m L water,with three triethylamine 1 ml being added,adjusted to p H 3. 0 with phosphoric acid) as mobile phase A,acetonitrile as mobile phase B,Gradient elution. The detection wavelength is 220 nm. With the flow rate of the mobile phase being 1. 0 m L/min and column temperature being 40 ℃,the sample volume is 10 μL. The results show that the separation degree between the main peak and impurity produced in different damaging conditions,as well as that between impurity and impurity is more than 1. 5,which means that complete separation can be achieved. The detection limits of impurity MAA6-1,MAA6-2,MAA7-3 and MAA6 are 0. 019,0. 013,0. 072,0. 108 ng respectively. There is a good linear relationship between the peak area and the concentration. The correction factor is 1. 0. It’s concluded that the method mentioned in this paper is simple,accurate,specific enough and suitable for the determination of the related substances in macitentan.更多还原