氢溴酸沃替西汀有关物质的测定方法

HPLC method for the determination of related substances in vortioxetine hydrobromide

目的建立氢溴酸沃替西汀中有关物质的测定方法。方法采用反相高效液相色谱法(HPLC),用Agilent HC-C18(2)色谱柱,流动相为乙腈-0.5%三乙胺溶液(用磷酸调至pH 6.0),梯度洗脱,检测波长226 nm,以外标法定量检测已知杂质,主成分自身对照法检测未知杂质。结果氢溴酸沃替西汀和杂质B、D、E、F、G、H、I、J、M等9个已知杂质的分离度良好;线性范围满足定量分析的要求,9个杂质的相关系数均在0.998以上;9个已知杂质的平均加样回收率在(100.2±1.1)%,RSD均<5%。结论反相高效液相色谱法具有高选择性(能定量分析9个工艺杂质及降解杂质),色谱条件简单易操作,高灵敏度、精密度良好,可作为氢溴酸沃替西汀原料杂质的控制方法。

Objective Reversed-phase high performance liquid chromatography(HPLC)was used with Agilent HC-C18(2)column.The mobile phase was acetonitrile-0.5%triethylamine solution(pH was adjusted to 6.0 with phosphoric acid),gradient elution,and detection wavelength was 226 nm.The known impurities were quantitatively detected by external standard method and unknown impurities were detected by principal component self-control method.ResultsThe separation of vortioxetine hydrobromide and nine known impurities B,D,E,F,G,H,I,J and M was good;the linear range met the requirement of quantitative analysis,and the correlation coefficient of 9 impurities were all above 0.998;the average recovery of nine known impurities was(100.2±1.1)%.RSD was less than 5%.Conclusion The method has high selectivity(can quantitatively analyze 9 kinds of process impurities and degradation of impurities),and the chromatographic conditions are simple and easy to operate,and the detection sensitivity is high and the precision is good,and it can be used as a control method for impurities in the raw material of vortioxetinehydrobromide.