UPLC MS/MS assay for routine quantification of dabigatran - A direct thrombin inhibitor - In human plasma
UPLC MS/MS assay for routine quantification of dabigatran - A direct thrombin inhibitor - In human plasma
复制标题
DOI：
10.1016/j.jpba.2011.09.018
复制
发表时间：
2012-01-25
影响因子：
3.4
通讯作者：
Basset, Thierry
中科院分区：
文献类型：
--
作者：
Delavenne, Xavier;Moracchini, Julie;Basset, Thierry
本文以[C-13(6)]-达比加群为内标，建立了快速、准确的液相色谱联用串联质谱法定量人血浆中达比加群的方法并进行了充分验证。血浆预处理包括一步甲醇蛋白沉淀。采用梯度洗脱方式，在Acquity UPLC BEH C8 100 mm × 1 mm × 1.7 μ m色谱柱上采用超高效反相色谱法进行分离。流动相为含有0.1%甲酸的蒸馏水和含有0.1%甲酸的甲醇的混合物。在正电喷雾电离中记录了特定的多重反应监测转变。该方法在2 ~ 500 μ g/L的浓度范围内呈线性。5、75、400 μ g/L的日内、日间精密度均在11.3%以下，精密度分别在93.8%和108.8%以内。定量下限为2 μ g/L。包括样品制备在内，总分析时间为10分钟。(C) 2011 Elsevier B.V.版权所有
This article described the development and full validation of rapid and accurate liquid chromatography method, coupled with tandem mass spectrometry detection, for quantification of dabigatran in human plasma with [C-13(6)]-dabigatran as internal standard. Plasma pretreatment involved a single step protein precipitation with methanol. Separation was performed by ultra performance reversed-phase chromatography on an Acquity UPLC BEH C8 100 mm x 1 mm x 1.7 mu m column using a gradient elution mode. The mobile phase was a mix of distilled water containing 0.1% formic acid and methanol containing 0.1% formic acid. Specific multiple reaction monitoring transitions were recorded in positive electrospray ionization. The method was linear over the concentration range of 2-500 mu g/L. The intra- and inter-day precision values were below 11.3% and accuracy was within 93.8% and 108.8% for all QC levels (5, 75 and 400 mu g/L). The lower limit of quantification was 2 mu g/L. Total analysis time was to 10 min including sample preparation. (C) 2011 Elsevier B.V. All rights reserved.