反相高效液相色谱法测定马西替坦有关物质

目的 建立马西替坦有关物质的反相高效液相色谱(RP-HPLC)测定方法.方法 采用Agilent C18柱(250 mm×4.6 mm,5 μm),以乙腈-水-甲酸(50:50:0.1)为流动相A,以乙腈-水-甲酸(85:15:0.1)为流动相B,梯度洗脱,流速为1.0 mL·min-1,检测波长为260 nm.结果 在选定色谱条件下,马西替坦与各杂质之间分离良好,杂质A、杂质B、杂质C、杂质D浓度分别在0.042~10.445 mg·L-1(r=1.000 0)、0.024~9.880 mg·L-1(r=1.000 0)、0.060~9.380 mg·L-1(r=0.999 5)、0.051~9.736 mg·L-1(r=1.000 0)范围内与峰面积呈良好的线性关系,上述杂质的平均回收率分别为99.91%、98.15%、98.51%、98.59%,RSD分别为1.61%、2.45%、3.89%、2.87%(n=9).结论 该方法专属性好,可用于测定马西替坦中的有关物质.

Determination of the related substances in macitentan by RP-HPLC

Objective To establish an RP-HPLC method for related substances of macitentan.Methods The determination was performed on an Agilent C18 column(250 mm×4.6 mm,5 μm);acetonitrile-water-formic acid(50:50:0.1)was used as mobile phase A and acetonitrile-water-formic acid(85:15:0.1)as mobile phase B by gradient elution.The flow rate and the detection wavelength were 1.0 mL·min-1 and 260 nm respectively.Results Under the selected chromatographic conditions,related substances were completely separated from macitentan.The calibration curves for impurity A,impurity B,impurity C,impurity D revealed good linearities over the ranges of 0.042-10.445 mg·L-1(r=1.000 0),0.024-9.880 mg·L-1(r=1.000 0),0.060-9.380 mg·L-1(r=0.999 5),and 0.051-9.736 mg·L-1(r=1.000 0),respectively.The recoveries of the above compounds were 99.91% with RSD of 1.61%,98.15% with RSD of 2.45%,98.51% with RSD of 3.89%,98.59% with RSD of 2.87%,respectively.Conclusion A specific method is established for the determination of macitentan-related substances.