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

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.