梯度洗脱HPLC法检查阿瑞匹坦原料药中的有关物质 |
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引用本文: | 于美芹,田兆兴,刘宝枚,罗兆亮. 梯度洗脱HPLC法检查阿瑞匹坦原料药中的有关物质[J]. 中国药房, 2014, 0(21): 1992-1995 |
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作者姓名: | 于美芹 田兆兴 刘宝枚 罗兆亮 |
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作者单位: | [1]日照市中医医院,山东日照276800; [2]河北大学药学院,河北保定071002 |
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摘 要: | 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。
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关 键 词: | 阿瑞匹坦 高效液相色谱法 梯度洗脱 有关物质 |
Determination of Related Substances in Aprepitant Raw Material by Gradient Elution HPLC |
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Affiliation: | YU Mei-qin, TIAN Zhao-xing, LIU Bao-mei, LUO Zhao-liang( 1.Rizhao Hospital of Traditional Chinese Medi- cine, Shandong Rizhao 276800, China; 2.School of Pharmacy, Hebei University, Hebei Baoding 071002, China) |
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Abstract: | 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. |
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Keywords: | Aprepitant HPLC Gradient elution Related substances |
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