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Research article
Open Access
A New High-Throughput LC-MS/MS Assay
for Therapeutic Level Monitoring of
Valproic Acid in Human Plasma
Laurian VLASE
1
, Daniela-Saveta POPA *
2
,
Dana MUNTEAN
1
, Sorin LEUCUTA
1
1
Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, “Iuliu Hatieganu”
University of Medicine and Pharmacy Emil Isac 13, RO-400023, Cluj-Napoca, Romania
2
Department of Toxicology, Faculty of Pharmacy, “Iuliu Hatieganu” University of Medicine and Pharmacy
Emil Isac 13, RO-400023, Cluj-Napoca, Romania
* Corresponding author. E-mail: dpopa@umfcluj.ro (D.-S. Popa)
Sci Pharm. 2008; 76: 663–671 doi:10.3797/scipharm.0808-12
Published: October 10
th
2008 Received: August 19
th
2008
Accepted: September 29
th
2008
This article is available from: http://dx.doi.org/10.3797/scipharm.0808-12
© Vlase et al; licensee Österreichische Apotheker-Verlagsgesellschaft m. b. H., Vienna, Austria.
This is an Open Access article distributed under the terms of the Creative Commons Attribution License
(http://creativecommons.org/licenses/by/3.0/), which permits unrestricted use, distribution, and reproduction
in any medium, provided the original work is properly cited.
Abstract
A new high-throughput liquid chromatographic tandem mass spectrometric (LC-
MS/MS) assay for the quantification of valproic acid in human plasma was
developed and validated. The separation was performed on a Zorbax SB-C18
column under isocratic conditions using a 48:52 (v/v) mixture of acetonitrile and
0.1% (v/v) acetic acid in water at 45 °C with a flow rate of 0.8 mL/min. The
detection of valproic acid was performed in SIM mode (m/z 143.1). The human
plasma samples (0.2 mL) were deproteinized with methanol and aliquots of 2 ȝL
from supernatants obtained after centrifugation were directly injected into the
chromatographic system. The method shows a good linearity (r > 0.9972),
precision (CV > 7.8 %) and accuracy (bias > 5.7 %) over the range of 5-200
ȝg/mL plasma. Lower limit of quantification (LLOQ) was 5 ȝg/mL and the
recovery was between 98-106 %. The method is not expensive, it needs a
minimum time for plasma sample preparation and has a run-time of 2.4 min for
instrument analysis (retention time of valproic acid was 1.8 min). The developed
and validated high-throughput method is very simple, rapid and efficient, with
wide applications in clinical level monitoring, pharmacokinetics and
bioequivalence studies.
Keywords
Valproic acid LC-MS/MS Therapeutic drug monitoring High-throughput assay