使用新型混合模式色谱柱HPLC法测定赖诺普利原料药中的三氟乙酸

Determination of Trifluoroacetic Acid in Lisinopril by HPLC with the New Mixed-Mode Column

目的:使用新型混合模式色谱柱高效液相色谱法测定赖诺普利原料药中的三氟乙酸。方法使用新型混合模式色谱柱(Thermo Acclaim Mixed-Mode WAX-1,250 mm×4.6 mm×5μm);以0.15 mol/L磷酸二氢钠溶液(用6 mol/L氢氧化钠溶液调节pH值至6.0)-甲醇-乙腈体积比80∶10∶10为流动相;柱温为30℃;流速为1.0 mL/min;检测波长为210 nm;进样量为50μL。结果:三氟乙酸在2.4985~99.9400μg/mL范围内线性关系良好(r=0.9999);检测限为0.7496μg/mL,定量限为2.4985μg/mL;加标回收率平均值为101.1%(RSD=0.59%,n=9)。结论:该方法准确、快速、方便,适用于赖诺普利原料药中三氟乙酸的测定。

Objective:To establish a HPLC method with the new mixed-mode column for determination of trifluoroacetic acid in lisinopril.Methods:HPLC with the new mixed-mode column(Thermo Acclaim Mixed-Mode WAX-1,250 mm×4.6 mm×5μm)(The temperature was 30℃)and 0.15 mol/L sodium dihydrogen phosphate solution(adjusted to pH 6.0 with 6mol/L NaOH solution):methanol:acetonitrile(80∶10∶10)as mobile phase were used.The flow rate was 1.0 mL·min-1,the detection wavelength was 210 nm and the injection volume was 50μL.Results:The calibration curve was well linear for trifluoroacetic acid in the range of 2.4985~99.9400μg/mL(r=0.9999).The LOD and LOQ were 0.7496μg/mL and 2.4985μg/mL,respectively.The average recovery was 101.1%,with RSD of 0.59%(n=9).Conclusion:The method is accurate,fast and convenient.It is suitable for the determination of trifluoroacetic acid in lisinopril.