摘要
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 [(13)C(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.
- 出版日期2012-1-25