高效液相色谱法测定埃索美拉唑镁肠溶片的有关物质

Determination of related substances of esomeprazole magnesium enteric-coated pellets-type tablets by gradient HPLC

目的:建立高效液相色谱梯度洗脱法测定埃索美拉唑镁肠溶片的有关物质。方法:采用venusil XBP C18色谱柱(250×4.6 mm,5μm),以乙腈-磷酸盐缓冲液(pH7.6)-水(10∶10∶80)为流动相A,以乙腈-磷酸盐缓冲液(pH7.6)-水(80∶1∶19)为流动相B进行梯度洗脱,流速为1 mL·min^(-1),柱温为25℃,检测波长为302 nm。结果:埃索美拉唑镁与杂质分离良好,埃索美拉唑镁、杂质D分别在0.50~5.02,0.50~4.96μg·mL^(-1)浓度范围内线性关系良好,检测限分别为1.25,2.50 ng·mL^(-1),定量限分别为5.00,6.25 ng·mL^(-1),埃索美拉唑镁与杂质D的平均回收率分别为99.91%,100.10%(n=9)。结论:该方法简便、准确、灵敏,专属性强,适用于埃索美拉唑镁肠溶片有关物质的测定。

OBJECTIVE To establish an method for the determination of related substances of esomeprazole magnesium enteric-coated pellets-type tablets by gradient HPLC.METHODS The separation was performed on a Venusil XBP C18column（250 mm×4.6 mm,5μm）,acetonitrile-phosphate buffered saline（pH7.6）-water（10∶10∶80）as mobile phase A,acetonitrilephosphate buffered saline（pH7.6）-water（80∶1∶19）as mobile phase B.The flow rate was 1 mL·min^-1,the column temperature was 25℃,the detection wavelength was at 302 nm.RESULTS The esomeprazole magnesium and related substances could be baseline separated.The calibration curves of esomeprazole magnesium and impurity D were linear in the concentration ranges of 0.50-5.02 and0.50-4.96 g·mL^-1.Their detection limit were 1.25 and2.50 ng·mL^-1,and their limit of quantification were5.00 and 6.25 ng·mL^-1,seperately.Their average recoveries were 99.91% and 100.10%（n=9）.CONCLUSION This method is rapid,accurate,sensitive,and can be used for the determination of the related substances of esomeprazole magnesium enteric-coated pellets-type tablets.