Development and validation of a UPLC-MS/MS method for quantitation of droxidopa in human plasma: Application to a pharmacokinetic study

作者：Wang, Haidong; Yang, Guangsheng; Zhou, Jinyu; Pei, Jiang; Zhang, Qiangfeng; Song, Xingfa; Sun, Zengxian^*

来源：Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2016, 1027: 234-238.

DOI：10.1016/j.jchromb.2016.04.056

• Droxidopa
• UPLC-MS/MS
• Plasma concentrations

In this study, a simple and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for quantitation of droxidopa in human plasma for the first time. A simple plasma protein precipitation method using methanol containing 3% formic acid was selected, and the separation was achieved by an Acquity UPLC (TM) BEH Amide column (2.1 mm x 50 mm, 1.7 mu m) with a gradient elution using acetonitrile, ammonium formate buffer and formic acid as mobile phase. The detection of droxidopa and benserazide (internal standard, IS) was performed using positive-ion electrospray tandem mass spectrometry via multiple reaction monitoring (MRM). The precursor-to-product ion transitions m/z 214.2 -> m/z 152.0 for droxidopa, and m/z 258.1 -> m/z 139.1 for IS were used for quantification. A lower limit of quantification of 5.00 ng/mL was achieved and the linear curve range was 5.00-4000 ng/mL using a weighted (1/x(2)) linear regression model. Intra-assay and inter-assay precision was less than 10.2%, and the accuracy ranged from 0.1% to 2.1%. Stability, recovery and matrix effects were within the acceptance criteria recommended by the regulatory bioanalytical guidelines. The method was successfully applied to a pharmacokinetic study of droxidopa in healthy Chinese volunteers.

• 出版日期2016-8-1
• 单位济宁医学院