A simple and rapid determination of valproic acid in human plasma using a non-porous silica column and liquid chromatography with tandem mass spectrometric detection.
A liquid chromatographic tandem mass spectrometric (LC-MS/MS) assay was developed and validated to determine valproic acid in human plasma. The method involved a solid-phase extraction of valproic acid and betamethasone valerate, an internal standard, from plasma and detection using an LC-MS/MS system with electrospray ionization source in negative ion mode. Separation was achieved within 3 min on a non-porous silica column with mobile phase containing ammonium acetate and methanol. Multiple reaction monitoring was utilized for detection monitoring at 142.89-142.89 for valproic acid and 457.21-457.21 for the internal standard. The calibration curve for valproic acid was linear over the range of 0.5-150 microg/mL. The limit of detection was 0.17 microg/mL and the lower limit of quantification was 0.5 microg/mL, when 0.2 mL plasma was used for extraction. The percentage coefficient of validation for accuracy and precision (inter- and intra-day) for this method was less than 9.5% with recovery ranging from 82.3 to 86.9% for valproic acid.
Matsuura
Katsuhiko
K
Department of Pharmacy, Gifu University Hospital, Gifu Pharmaceutical University, Gifu, Japan.
Ohmori
Tomofumi
T
Nakamura
Mitsuhiro
M
Itoh
Yoshinori
Y
Hirano
Kazuyuki
K
D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014635:Valproic Acid / Q000097:blood*
D014635:Valproic Acid; D012822:Silicon Dioxide