RP-HPLC法检测阿齐沙坦有关物质的方法改进  

Improvement of Determination on the Related Substances in Azilsartan by RP-HPLC

作　　者：张丽 刘发贵 杨丹丹 李敏 刘思光 张贵民 ZHANG Li;LIU Fa-gui;YANG Dan-dan;LI Min;LUI Si-guang;ZHANG Gui-min(National Engineering Research Center of Chiral Drugs,Lunan Pharmaceutical Group,Linyi 273400,China)

机构地区：[1]鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂276002

出　　处：《海峡药学》2023年第5期60-62,共3页Strait Pharmaceutical Journal

摘　　要：目的建立一种新的阿齐沙坦有关物质检测方法。方法以YMC Triart C 18(4.6×250 mm,5μm)为色谱柱;以0.05 mol·L^(-1)乙酸铵缓冲液(氨水调节pH至9.0)为流动相A,甲醇为流动相B,线性梯度洗脱;流速0.8 mL·min^(-1);检测波长251 nm。结果阿齐沙坦与各杂质分离良好,各杂质和阿齐沙坦质量浓度0.1~1.0μg·mL^(-1)范围内,浓度与峰面积呈良好的线性关系,相关系数0.9990~1.0000;1、2、3、4和5检测限分别为0.0476、0.0570、0.0532、0.0588和0.0556μg·mL^(-1),平均回收率分别为96.66%、109.94%、102.18%、100.62%和100.26%,RSD分别为5.53%、6.14%、1.45%、3.0%和3.48%(n=9)。结论本法专属、可靠,可用于阿齐沙坦原料药有关物质的测定。OBJECTIVE To establish a new method for the determination of related substances in azilsartan by RP-HPLC.METHODS The determination was performed on a YMC Triart C 18 column(4.6×250 mm,5μm)and the mobile phase A consisted of 0.5 mol·L^(-1) ammonium acetate buffer solution(adjust pH to 9.0 with ammonium hydroxide),the mobile phase B consisted of methanol.Linear gradient elution.The detection wavelength and flow rate was 251 nm and 0.8 mL·min^(-1) respectively.RESULTS An excellent separation was achieved for related substances in azilsartan under the above chromatographic conditions.The calibration cures for azilsartan and its related substances revealed good linearities over the ranges of 0.1-1.0μg·mL^(-1),the correlation coefficient was 0.9990-1.0000.The LOD of 1,2,3,4,5 was 0.0476μg·mL^(-1),0.0570μg·mL^(-1),0.0532μg·mL^(-1),0.0588μg·mL^(-1),0.0556μg·mL^(-1),average recovery was 99.66%,109.94%,102.18%,100.62%,100.26%respectively and the RSD was 5.53%,6.14%,1.45%,3.0%,3.48%(n=9).CONCLUSION The method was accurate and sensitive for separation and detection related substances in azilsartan.

关 键 词：RP-HPLC 有关物质 阿齐沙坦 

分 类 号：R927[医药卫生—药学]