Sensitive liquid chromatography tandem mass spectrometry method for the quantification of sitagliptin, a DPP-4 inhibitor, in human plasma using liquid-liquid extraction.
Sensitive liquid chromatography tandem mass spectrometry method for the quantification of sitagliptin, a DPP-4 inhibitor, in human plasma using liquid-liquid extraction.
复制标题
DOI：
10.1002/bmc.926
复制
发表时间：
2008-02
期刊：
影响因子：
--
通讯作者：
R. Nirogi;V. Kandikere;K. Mudigonda;Prashanth Komarneni;R. Aleti;R. Boggavarapu
中科院分区：
文献类型：
--
作者：
R. Nirogi;V. Kandikere;K. Mudigonda;Prashanth Komarneni;R. Aleti;R. Boggavarapu
开发并验证了一种灵敏的高效液相色谱-正离子电喷雾串联质谱法，用于定量人血浆中DPP-4抑制剂西格列汀。液-液萃取后，在反相色谱柱上使用等度移动的相分离分析物，并在多反应监测模式下使用相应的[M + H]（+）离子（西格列汀为m/z 408-235，内标物为m/z 310-148）通过MS/MS进行分析。该测定法显示人血浆中西格列汀的线性动态范围为0.1-250 ng/mL。定量下限为0.1 ng/mL，相对标准偏差小于6%。对于标准曲线范围内的浓度，获得了可接受的精密度和准确度。每个样品的运行时间为2.0分钟，每天可以分析300多个人血浆样品。经验证的方法已成功用于分析人血浆样品，以应用于药代动力学研究。
A sensitive high-performance liquid chromatography-positive ion electrospray tandem mass spectrometry method was developed and validated for the quantification of sitagliptin, a DPP-4 inhibitor, in human plasma. Following liquid-liquid extraction, the analytes were separated using an isocratic mobile phase on a reverse-phase column and analyzed by MS/MS in the multiple reaction monitoring mode using the respective [M + H](+) ions, m/z 408-235 for sitagliptin and m/z 310-148 for the internal standard. The assay exhibited a linear dynamic range of 0.1-250 ng/mL for sitagliptin in human plasma. The lower limit of quantification was 0.1 ng/mL with a relative standard deviation of less than 6%. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 2.0 min for each sample made it possible to analyze more than 300 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic studies.