巯嘌呤口服混悬液有关物质的HPLC法测定

Determination of Related Substances in Thiopurine Oral Suspension by HPLC

建立了HPLC法测定巯嘌呤口服混悬液中的有关物质,以加校正因子的自身对照法定量。采用Uitimate Phenyl-Ether色谱柱,以0.04%甲酸∶甲醇为流动相,等度洗脱,检测波长260 nm。计算有关物质的相对校正因子(RCF),以此计算有关物质含量,并与对照品法测定结果比较,以验证方法的准确性。结果主成分巯嘌呤与相邻杂质,以及各杂质之间均分离良好,RCF法与对照品法测定结果无显著性差异。已知杂质2、3的相对保留时间分别为0.56和4.33,相对校正因子分别为0.16和0.23,2和3的平均加样回收率为104.2%和95.3%,RSD为3.2%和2.9%。本方法重复性好、灵敏度高,适用于巯嘌呤口服混悬液中有关物质的分析。

a hplc method was established for the determination of related substances in mercaptopurine oral suspension,with self-control method added with correction factors.A Uitimate Phenyl-Ether chromatographic column was used with 0.04%formic acid:methanol as mobile phase,and the detection wavelength was 260nm.The relative correction factor(RCF)of related substances is calculated to calculate the content of related substances,and compared with the determination results of the reference substance method to verify the accuracy of the method.Results The main component mercaptopurine was well separated from its neighboring impurities,and there was no significant difference between RCF method and control method.It is known that the relative retention times of impurities 2 and 3 are 0.56 and 4.33 respectively,the relative correction factors are 0.16 and 0.23 respectively,and the average recovery rates of impurities 2 and 3 are 104.2%and 95.3%,RSD are 3.2%and 2.9%.The method has good repeatability and high sensitivity,and is suitable for the analysis of related substances in mercaptopurine oral suspension.