SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM

Valproic acid (VPA) is one of the mostly used antiepileptic drugs that may have some side effects so, it is highly recommended to evaluate its serum concentrations. The aim of this study was to develop a simple, fast and economic method using gas-chromatography equipped with flame ionization detecto...

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Main Authors: H. R. Falahat-Pisheh, T. R. Neyestani M. Bigdeli
Format: Article
Language:English
Published: Tehran University of Medical Sciences 2007-04-01
Series:Acta Medica Iranica
Subjects:
Online Access:https://acta.tums.ac.ir/index.php/acta/article/view/3248
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author H. R. Falahat-Pisheh
T. R. Neyestani M. Bigdeli
author_facet H. R. Falahat-Pisheh
T. R. Neyestani M. Bigdeli
author_sort H. R. Falahat-Pisheh
collection DOAJ
description Valproic acid (VPA) is one of the mostly used antiepileptic drugs that may have some side effects so, it is highly recommended to evaluate its serum concentrations. The aim of this study was to develop a simple, fast and economic method using gas-chromatography equipped with flame ionization detector (GC/FID) and VPA analysis. To do this, 200 µl of serum was mixed with an aliquot of caproic acid (200 µL, methanolic solution) as internal standard and extracted by stepwise addition of hydrochloric acid and chloroform with slight agitation between each step. After centrifugation, 1.0 µl of the bottom layer was injected into a wide-bore nonpolar capillary column. Injectable samples for analysis of unbonded VPA were prepared by ultra filtration followed by solid phase extraction (SPE). Caproic acid and VPA were eluted after 1.5 min and 3.0 min, respectively (total GC run time about 3.2 minutes). This GC/FID method was linear over a range of 2.5-6400 µg/ml with the mean recovery of 92%. The intra- and inter-assay precision in the range of 25-100 µg/ml was 1.50-, 2.95, and 2.35- 3.22%, respectively. The simplicity of sample preparation with no derivatization, short run-time and high sensitivity sufficient to detect low concentrations of the drug makes this method suitable for research as well as routine use.
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spelling doaj.art-be094b5c93414593b5bab58ffd9df3952022-12-22T01:46:18ZengTehran University of Medical SciencesActa Medica Iranica0044-60251735-96942007-04-01452SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM H. R. Falahat-Pisheh0 T. R. Neyestani M. Bigdeli1 Valproic acid (VPA) is one of the mostly used antiepileptic drugs that may have some side effects so, it is highly recommended to evaluate its serum concentrations. The aim of this study was to develop a simple, fast and economic method using gas-chromatography equipped with flame ionization detector (GC/FID) and VPA analysis. To do this, 200 µl of serum was mixed with an aliquot of caproic acid (200 µL, methanolic solution) as internal standard and extracted by stepwise addition of hydrochloric acid and chloroform with slight agitation between each step. After centrifugation, 1.0 µl of the bottom layer was injected into a wide-bore nonpolar capillary column. Injectable samples for analysis of unbonded VPA were prepared by ultra filtration followed by solid phase extraction (SPE). Caproic acid and VPA were eluted after 1.5 min and 3.0 min, respectively (total GC run time about 3.2 minutes). This GC/FID method was linear over a range of 2.5-6400 µg/ml with the mean recovery of 92%. The intra- and inter-assay precision in the range of 25-100 µg/ml was 1.50-, 2.95, and 2.35- 3.22%, respectively. The simplicity of sample preparation with no derivatization, short run-time and high sensitivity sufficient to detect low concentrations of the drug makes this method suitable for research as well as routine use.https://acta.tums.ac.ir/index.php/acta/article/view/3248gas-chromatography
spellingShingle H. R. Falahat-Pisheh
T. R. Neyestani M. Bigdeli
SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
Acta Medica Iranica
gas-chromatography
title SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
title_full SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
title_fullStr SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
title_full_unstemmed SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
title_short SIMPLE AND RAPID GAS-CHROMATOGRAPHIC METHOD FOR QUANTITATION OF TOTAL AND FREE VALPROIC ACID IN HUMAN SERUM
title_sort simple and rapid gas chromatographic method for quantitation of total and free valproic acid in human serum
topic gas-chromatography
url https://acta.tums.ac.ir/index.php/acta/article/view/3248
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