HPLC测定马西替坦中的有关物质

目的 采用HPLC法测定马西替坦中有关物质的含量.方法 色谱柱为AgelaVenusil XBP C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(1L水中加入1.0 mL三乙胺,用磷酸调pH3),梯度洗脱,流速1 mL· min-1,柱温35℃,检测波长220nm,进样量10 μL.结果 马西替坦与11种杂质均可达到基线分离,马西替坦和各杂质的线性范围均为0.05～1.5 μg·mL-1,重复性试验的RSD＜ 2.0％,平均回收率的RSD＜ 10％.结论 所用方法专属性强、准确度高,可用于马西替坦中有关物质的检查.

Determination of the related substances in Macitentan by HPLC

OBJECTIVE To establish an HPLC method to determine the related substances in Macitentan.METHODS Analysis was carried out on an AgelaVenusil XBP C18column(250 mm × 0.46 mm) using acetonitrile-water(1 mL of triethylamine with 1 L water) as the mobile phase.The detection wavelength was 220 nm with the flow rate of 1 mL·min-1.Column temperature was maintained at 35 ℃ and the injection volume was 10 μL.RESULTS The calibration curve was linear within the range of 0.05-1.5 μg·mL-1 of Macitentan and impurities.The RSD of repeatability tests was less than 2.0％,and the RSD of recovery rate was less than 10％.CONCLUSION The method is simple,specific,accurate and suitable for analyzing the related substances in Macitentan.