Rapid,simple,specific liquid chromatographic-electrospray mass spectrometry method for the determination of glibenclamide in human plasma

摘要

A sensitive liquid chromatographic-electrospray ionization mass spectrometric method was developed and validated for fast determination of glibenclamide in human plasma.After deprotienation with methanol,centrifugation,evaporation to dryness and dissolving in mobile phase,samples were separated using a Hypersil-Keystone C18 reversed-phase column (150mmX2.1 mm ID,5mum),together with a mobile phase containing of acetonitrile-10 mM ammonium acetate (55:45,v/v),0.2% acetic acid and 0.1 % trifluoracetic acid.Glibenclamide and its internal standard,glipizide,were measured by electrospray ion source in positive selective ion monitoring mode.The method demonstrated linearity from 1 to 400ng/mL (r=0.998).The limit of quantification for glibenclamide in plasma was 1 ng/mL with good accuracy and precision.The recovery of the method was over 91.5%.Intra- and inter-day precision ranged from 3.42 to 5.57 and 7.49 to 8.64% (RSD),respectively.