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首页> 外文期刊>Journal of mass spectrometry: JMS >A liquid chromatography-tandem mass spectrometry method for the simultaneous determination of exemestane and its metabolite 17-dihydroexemestane in human plasma
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A liquid chromatography-tandem mass spectrometry method for the simultaneous determination of exemestane and its metabolite 17-dihydroexemestane in human plasma

机译：液相色谱-串联质谱法同时测定人血浆中的依西美坦及其代谢产物17-二氢依西美坦

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摘要

A simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitation of exemestane (Exe) and its main metabolite 17-dihydroexemestane (DhExe) in human plasma. The analytes were extracted by protein precipitation with acetonitrile, containing stable C-13-labelled Exe (C-13(3)-Exe) as internal standard, and measured by LC-MS/MS. The best chromatographic separationof the analytes from the interferences was achieved by using a Phenyl column operating under isocratic regime conditions. The total chromatographic runtime was 5.0 min and the elution of Exe and DhExe occurred at 2.5 min and 2.9 min, respectively. Quantitation was performed by employing the positive electrospray ionization (ESI) technique and multiple reaction monitoring mode (MRM). The monitored precursor to product-ion transitions for Exe, DhExe and C-13(3)-Exe internal standard were m/z 297.0 -> 120.8, m/z 299.1 -> 134.9 and m/z 300.0 -> 123.2, respectively. The lower limit of quantitation (LLOQ) was 0.1 ng/ml for DhExe and 0.2 ng/ml for Exe. The method was linear up to 36-51 ng/ml with r(2) >= 0.998. The intra- and inter-assay precision were <= 7.7% and 5.1% for Exe and >= 8.1 and 4.9% for DhExe while deviations from nominal values were in the 1.5-13.2% and -9.0-5.8% ranges for Exe and DhExe, respectively. The analytical method resulted robust and suitable for pharmacokinetic monitoring of Exe and its main metabolite during adjuvant therapy in patients with breast cancer.
机译：已经开发了一种简单灵敏的液相色谱-串联质谱（LC-MS / MS）方法，并已用于定量人体血浆中的依西美坦（Exe）及其主要代谢物17-二氢依西美坦（DhExe）。通过用含有稳定的C-13标记的Exe（C-13（3）-Exe）作为内标的乙腈进行蛋白质沉淀来提取分析物，并通过LC-MS / MS进行测量。通过使用在等度条件下运行的苯基色谱柱，可以最佳地分离分析物与干扰物。总色谱运行时间为5.0分钟，Exe和DhExe的洗脱时间分别为2.5分钟和2.9分钟。通过采用正电喷雾电离（ESI）技术和多反应监测模式（MRM）进行定量。监测的Exe，DhExe和C-13（3）-Exe内标到产物离子跃迁的前体分别为m / z 297.0-> 120.8，m / z 299.1-> 134.9和m / z 300.0-> 123.2。 DhExe的定量下限（LLOQ）为0.1 ng / ml，Exe的定量下限（LLOQ）为0.2 ng / ml。该方法线性高达36-51 ng / ml，r（2）> = 0.998。对于Exe，测定内和测定间精度分别为<= 7.7％和5.1％，对于DhExe，分别为> = 8.1和4.9％，而对于Exe和DhExe，其与标称值的偏差在1.5-13.2％和-9.0-5.8％范围内， 分别。该分析方法结实耐用，适用于乳腺癌患者辅助治疗期间Exe及其主要代谢产物的药代动力学监测。

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