作者: Haidong Wang , Guangsheng Yang , Jinyu Zhou , Jiang Pei , Qiangfeng Zhang
DOI: 10.1016/J.JCHROMB.2016.04.056
关键词: Analytical chemistry 、 Electrospray 、 Ammonium formate 、 Selected reaction monitoring 、 Mass spectrometry 、 Droxidopa 、 Tandem mass spectrometry 、 Detection limit 、 Chemistry 、 Chromatography 、 Formic acid
摘要: In this study, a simple and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed validated for quantitation of droxidopa in human plasma the first time. A protein precipitation using methanol containing 3% formic acid selected, separation achieved by an Acquity UPLC™ BEH Amide column (2.1mm×50mm, 1.7μm) with gradient elution acetonitrile, ammonium formate buffer as mobile phase. The detection benserazide (internal standard, IS) performed positive-ion electrospray tandem via multiple reaction monitoring (MRM). precursor-to-product ion transitions m/z 214.2→m/z 152.0 droxidopa, 258.1→m/z 139.1 IS were used quantification. lower limit quantification 5.00ng/mL linear curve range 5.00-4000ng/mL weighted (1/x(2)) regression model. Intra-assay inter-assay precision less than 10.2%, accuracy ranged from 0.1% to 2.1%. Stability, recovery matrix effects within acceptance criteria recommended regulatory bioanalytical guidelines. successfully applied pharmacokinetic study healthy Chinese volunteers.