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    STUDIA CHEMIA - Ediţia nr.1 din 2013  
         
  Articol:   DETERMINATION OF METHYLDOPA IN HUMAN PLASMA BY LC/MS-MS FOR THERAPEUTIC DRUG MONITORING.

Autori:  LAURIAN VLASE, DAN MIHU, ADINA POPA. 		 
       
         
  Rezumat:  A simple and rapid liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) method for therapeutic level monitoring of methyldopa in human plasma was developed and validated. The separation was performed on a Zorbax SB-C18 column under isocratic conditions using a mobile phase of 2:98 (v/v) acetonitrile and 0.2% (v/v) formic acid in water at 40ºC with a flow rate of 0.8 mL/min. The detection of was performed using an ion trap MS with electrospray positive ionisation in multiple reaction monitoring (MRM) mode (m/z 212.1 →139.2, 166.2, 195.2). The human plasma samples (0.2 mL) were deproteinised with methanol and aliquots of 1.5 μL from supernatants obtained after centrifugation were directly injected into the chromatographic system. The method shows a good linearity, precision (CV < 8.4 %) and accuracy (bias < 11.1 %) over the range of 0.32-20.48 μg/mL plasma. The lower limit of quantification (LLOQ) was 0.32 μg/mL and the recovery was between 90.9-101.4 %. The method is fast, with a minimum time for plasma sample preparation and a run-time of 1.5 min for instrument analysis (retention time of methyldopa was 1.05 min). The developed and validated method is simple, rapid, selective and sufficiently sensitive to be applied in clinical level monitoring, pharmacokinetics or bioequivalence studies of methyldopa.

Keywords: methyldopa, LC/MS-MS, therapeutic drug monitoring 		 
         
     
         
         
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