高效液相色谱法测定阿奇沙坦的含量和有关物质  

HPLC determination of azilsartan content and its related substances

作　　者：顾维钧 侯玉婷 杨明华 孙雪妹 隋强[2] 唐超[2] 

机构地区：[1]上海市浦东食品药品检验所,上海201203 [2]上海医药工业研究院,上海200437

出　　处：《药物分析杂志》2014年第12期2185-2191,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定阿奇沙坦含量及有关物质的HPLC法。方法:采用反相高效液相色谱法,测定其含量和有关物质,以阿奇沙坦为参照物,分别计算阿奇沙坦杂质A^F相对保留时间及相对校正因子。色谱条件:采用Waters CSH C18色谱柱(4.6mm×150 mm,5μm),以0.1%磷酸为流动相A,乙腈为流动相B,线性梯度洗脱,流速1.0 m L·min-1,柱温35℃,检测波长为248 nm。结果:阿奇沙坦与各杂质峰均分离良好,阿奇沙坦与各已知杂质A^F在各自线性范围内线性关系良好(r=0.9999);阿奇沙坦平均加样回收率(n=3)分别为100.8%、100.7%、100.7%,RSD分别为1.1%、0.6%、0.7%;最低定量限按S/N≈10计算,定量限均为0.4μg·m L-1;最低检测限按S/N≈3计算,检出限均为0.12μg·m L-1;3批样品含量测定结果分别为100.2%、99.91%和101.1%。供试品溶液12 h内稳定。结论:方法学验证表明所建立的方法符合定量测定阿奇沙坦含量和杂质的要求,适用于阿奇沙坦和杂质的质量控制。Objective： To establish an HPLC method to determine azilsartan content and its related substances. Methods： Azilsartan and the related substances were determined by RP - HPLC. The impurities A - F in azilsar- tan,the relative retention times and the relative correction factors were determined respectively by HPLC with azil- sartan as the reference substance. The chromatographic condition was as follows. The Waters CSH C18 column （4.6 mm × 150 mm,5 μm）was adopted, the mobile phase was 0. 1% phosphoric acid （A） - acetonitrile（ B ）with gradi- ent elution at a flow rate of 1.0 mL ·min^- 1, the column temperature was 35 %, and the detection wavelength was 248 nm. Results： Azilsartan and the impurities were separated well. The calibration curves of six impurities were lin- ear in each concentration range （ r = 0. 9999 ）. The average recovery （ n = 3 ） of azilsartan was 100. 8% , 100. 7%, 100.7% and RSD was 1.1% ,0. 6% ,0.7% ,respectively. The limits of quantification of impurities was 0.4 μg · mL^-1 and the limit of detection was 0. 12 μg · mL^-1. The content determination results for the 3 batches of samples were 100.2% ,99.91% and 101.1% ,respectively. The solution was stable for 12 h. Conclusion： The validation test showed that the proposed method met the requirements for the intended analytical applications, and the method can be used for quality control of azilsartan.

关 键 词：阿奇沙坦 阿奇沙坦杂质A^F 杂质结构 高效液相色谱法 梯度洗脱 

分 类 号：R917[医药卫生—药物分析学]