梯度洗脱HPLC法检查阿瑞匹坦原料药中的有关物质

目的:建立检查阿瑞匹坦原料药中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Merck C18;流动相A为0.2%磷酸溶液(pH 2.5),流动相B为乙腈,梯度洗脱;检测波长为215 nm。按照加校正因子主成分自身对照法进行定量计算。结果:起始原料Ⅰ、起始原料Ⅱ、中间体Ⅰ、中间体Ⅱ、阿瑞匹坦各峰之间均能达到很好的分离,并在各自的检测质量浓度范围内线性关系良好(r=0.999 0⁰.999 8),检测限分别为0.01、0.06、0.01、0.25、0.03μg/ml;各杂质平均回收率分别为99.43%、99.05%、98.85%、100.6%(RSD为0.29%、0.10%、0.64%、0.26%,n=3)。结论:本文建立的方法灵敏快速、准确可靠,可作为阿瑞匹坦原料药的有关物质检查方法。

Determination of Related Substances in Aprepitant Raw Material by Gradient Elution HPLC

OBJECTIVE：To establish a method for the determination of related substances in aprepitant raw material.METHODS：Gradient elution HPLC method was adopted.The analysis was performed on Merck C18column with mobile phase A composed of 0.2% phosphoric acid solution（pH 2.5）and mobile phase B consisted of acetonitrile（gradient elution）.The detection wavelength was set at 215 nm.The related substances were determined by the self-control method with corrected factor.RESULTS：Starting material Ⅰ,starting material Ⅱ,intermediatesⅠ,intermediatesⅡ and aprepitant were completely separated from the main peak.The calibration curve of these related substances were in good linear relationship（r=0.999 0-0.999 8）,and the limits of detection were 0.01,0.06,0.01,0.25 and 0.03 μg/ml,respectively.The average recoveries of the impurities mentioned above were 99.43%（RSD=0.29%,n=3）,99.05%（RSD=0.10%,n=3）,98.85%（RSD=0.64%,n=3）and 100.6%（RSD=0.26%.n= 3）,respectively.CONCLUSIONS：The developed method is sensitive,rapid,accurate and reliable,and can be used for the detection of related substances in aprepitant raw material.