HPLC法测定复方制剂厄贝沙坦氢氯噻嗪片有关物质

Determination of Related Substances of Irbesartan and Hydrochlorothiazide Tablets by HPLC

目的:建立厄贝沙坦氢氯噻嗪片有关物质检测方法。方法:采用Phenomenex Luna®3μm CN 100A(4.6 mm×150 mm,3μm)为色谱柱;以0.01 mol·L^(-1)的磷酸二氢钾缓冲液(取磷酸二氢钾1.36 g,加水1000 mL溶解,加入2 mL三乙胺,用磷酸调节pH值至3.0)为流动相A,以甲醇-乙腈(5∶1)为流动相B,线性梯度洗脱0~5 min,流动相B 18%;5~22min,流动相B 18%~45%;22~27 min,流动相B 45%;27~28 min,流动相B 45%~18%;流速为1.0 mL·min^(-1),检测波长为220 nm。结果:各已知杂质在限度质量分数10%~200%范围内线性关系良好,r≥0.9999,各杂质及主峰与相邻杂质分离良好;各已知杂质的回收率在98.0%~110.6%范围内,RSD均小于2.0%(n=12);溶液在24 h内稳定;精密度和重复性RSD均小于5.0%。结论:方法精密度好、准确度高,可用于本品的有关物质检测。

A HPLC method for the determination of the related substances of Irbesartan and Hydrochlorothiazide Tablets was established.The column was Phenomenex Luna®3μm CN 100A(4.6 mm×150 mm,3μm),with the mobile phase A of 0.01 mol·L^(-1) potassium dihydrogen phosphate(adding 2 mL trimethylamine to the 1000 mL solution,and adjusting the pH to 3.0 with phosphoric acid),and the mobile phase B of methanol-acetonitrile(5∶1).The linearity gradient elution was as follows:0~5 min,mobile B 18%;5~22 min,mobile B 18%~45%;22~27 min,mobile B 45%;27~28 min,mobile B 45%~18%.The flow rate was 1.0 mL·min^(-1),and the detection wavelength was 220 nm.The good linearity for related substances was obtained over the range of 10%~200%(r≥0.9999).The main substance and its impurities could be well separated.The recovery of related substances was 98.0%~110.6%(RSD<2.0%,n=12).The solution was stable within 24 h,and the RSDs of precision and repeatability were less than 5.0%.The method has good precision and high accuracy,and can be used for the detection of related substances in Irbesartan and Hydrochlorothiazide Tablets.