论文部分内容阅读
目的 建立一种测定人血浆中利格列汀浓度的液相色谱-串联质谱法.方法 用蛋白沉淀法处理样品,色谱柱:AQ-C18HP(2.1 mm×100.0 mm,3.0 μm),流动相:100%水含10 mmol· L-1醋酸铵和0.1%甲酸-95%乙腈含0.1%甲酸,流速:0.40 mL· min-1,柱温:40 ℃,进样量:15.0 μL.考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应及稳定性.结果 利格列汀在0.05～25.00 ng· mL-1内线性关系良好,标准曲线为y=9.35×10 -2x+1.88×10 -4(r=0.998 2),定量下限为0.05 ng· mL-1,日内和日间的RSD均小于10.0%,提取回收率在103.8%以上.结论 本方法简便快速,准确度高,灵敏度好,适用于人血浆中利格列汀的浓度测定.“,”Objective To establish a HPLC-MS/MS method to deter-minate the concentration of linagliptin in human plasma .Methods The samples were treated by protein precipitation method .The chromato-graphic column was AQ-C18HP (2.1 mm×100.0 mm,3.0 μm), mo-bile phase was 100%water contained with 10 mmol· L-1ammonium ac-etate and 0.1% formic acid -95% acetonitrile contained with 0.1%formic acid, flow rate was 0.40 mL· min -1, column temperature was 40℃, injection volume was 15.0 μL, mobile phase. The specificity, standard curve and lower limit of quantitation , precision and recovery, matrix effect and stability of the method were investigated .Results The standard curve of metformin was y=9.35 ×10 -2x +1.88 ×10 -4( r =0.998 2), and linagliptin had good linear relationship in 0.05 -25.00 ng· mL-1.The limit of quantification was 0.05 ng· mL-1.The intra-day RSD and inter-day RSD were less than 10.0%, respectively.The recovery rate of extraction was over 103.8%.Conclusion The method is simple, rapid, accurate and sensitive , which is suitable for the deter-mination of linagliptin in human plasma .