Small molecule adduct formation with the components of the mobile phase as a way to analyse valproic acid in human serum with liquid chromatography-tandem mass spectrometry.

作者: Marek Dziadosz , Michael Klintschar , Jörg Teske

DOI: 10.1016/J.JCHROMB.2014.03.033

关键词: Acetic acidSodium acetateLiquid chromatography–mass spectrometryAdductChemistryAmmonium acetateDetection limitMass spectrometryChromatographyProtein precipitation

摘要: Abstract A valproic acid (VPA) LC-MS/MS analytical method using analyte adduct formation was developed and validated in human serum. The fragmentation of the sodium acetate (mass transition: 225/143) acetic 203/143) were used as target qualifier mass transition, respectively. Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm column a mobile phase consisting (H2O/methanol = 95/5, v/v) B (H2O/methanol = 3/97, v/v), both with 10 mM ammonium 0.1% (pH = 3.2) used. binary flow pumping mode total rate 0.4 mL/min applied. Protein precipitation 1 mL sample preparation. calculated limit detection/quantification 0.45/1.0 μg/mL inter-/intra-day precision

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