| 吴标,李晓梅,崔红晓.反相高效液相色谱法测定马西替坦有关物质[J].安徽医药,2017,21(2):248-251. |
| 反相高效液相色谱法测定马西替坦有关物质 |
| Determination of the related substances in macitentan by RP-HPLC |
| 投稿时间：2016-07-04 |
| DOI： |
| 中文关键词: 马西替坦 反相高效液相色谱法 有关物质 |
| 英文关键词: Macitentan RP-HPLC Related substances |
| 基金项目: |
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| 摘要点击次数: 2343 |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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 Aand acetonitrile-water-formic acid(85∶15∶0.1)as mobile phase Bby 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 Drevealed 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. |
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