Acta Pharm. 62 (2012) 211-220
Original research paper
Development and validation of a bioanalytical
LC-UV method with solid-phase extraction for determination of valproic acid in
saliva
JASMINA
TONIC-RIBARSKA, ARLINDA HAXHIU, ZORAN STERJEV, GORDANA KITEVA,
LjUBICA SUTURKOVA and SUZANA TRAJKOVIC-JOLEVSKA
jasminatonic@yahoo.com
1 Institute of
Applied Chemistry and Pharmaceutical Analysis, Faculty of Pharmacy, University
Ss Cyril and Methodius , Skopje, Macedonia
2 Department of
Pharmacy, Medical Sciences Faculty, State University of Tetova, Tetovo,
Macedonia
3 Institute of
Pharmaceutical Chemistry, Faculty of Pharmacy, University Ss Cyril and
Methodius , Skopje, Macedonia
4 Clinic
of Neurology, Faculty of Medicine, University Ss Cyril and Methodius , Skopje,
Macedonia
Accepted April 5, 2012
A bioanalytical HPLC method with UV detection for the determination of the antiepileptic drug valproic acid in human saliva has been developed and validated. Saliva represents an alternative matrix for monitoring of antiepileptic drugs due to the increasing interest in free drug concentration. The proposed method involved solid-phase extraction for sample preparation and yielded very good mean recoveries of 99.4 % and 97.9 % for valproic acid and IS, respectively. The calibration function for valproic acid was linear over the concentration range of 1.0 50.0 g mL-1 (R2 = 0.9989). Within-run and between-run precision and accuracy were studied at four concentrations and RSDs were less than 7.3 and 2.2 %, while accuracy values were higher than 96.8 and 97.5 %, respectively. The described method provides sensitivity, linearity, precision, accuracy and is suitable for analyses of valproic acid in saliva samples.
Keywords: valproic acid, saliva, solid-phase extraction, high-performance
liquid chromatography, validation