Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical...

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Main Authors: Greyce Kelly Steinhorst Alcantara, Leandro Augusto Calixto, Luiz Alberto Beraldo de Moraes, Regina Helena Costa Queiroz, Anderson Rodrigo Moraes de Oliveira, Cristiane Masetto de Gaitani
Format: Article
Language:English
Published: Wiley 2016-01-01
Series:Journal of Analytical Methods in Chemistry
Online Access:http://dx.doi.org/10.1155/2016/5976324
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author Greyce Kelly Steinhorst Alcantara
Leandro Augusto Calixto
Luiz Alberto Beraldo de Moraes
Regina Helena Costa Queiroz
Anderson Rodrigo Moraes de Oliveira
Cristiane Masetto de Gaitani
author_facet Greyce Kelly Steinhorst Alcantara
Leandro Augusto Calixto
Luiz Alberto Beraldo de Moraes
Regina Helena Costa Queiroz
Anderson Rodrigo Moraes de Oliveira
Cristiane Masetto de Gaitani
author_sort Greyce Kelly Steinhorst Alcantara
collection DOAJ
description Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.
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spelling doaj-art-c5feb7db8ce84dd19b9dca9702fc279f2025-02-03T07:25:36ZengWileyJournal of Analytical Methods in Chemistry2090-88652090-88732016-01-01201610.1155/2016/59763245976324Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass SpectrometryGreyce Kelly Steinhorst Alcantara0Leandro Augusto Calixto1Luiz Alberto Beraldo de Moraes2Regina Helena Costa Queiroz3Anderson Rodrigo Moraes de Oliveira4Cristiane Masetto de Gaitani5Department of Pharmaceutical Sciences, Faculty of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, 14040-903 Ribeirão Preto, SP, BrazilDepartment of Exact and Earth Sciences, Institute of Environmental, Chemical and Pharmaceutical Sciences, Federal University of São Paulo, 09972-270 Diadema, SP, BrazilDepartament of Chemistry, Faculty of Philosophy, Sciences and Letters of Ribeirão Preto, University of São Paulo, 14040-901 Ribeirão Preto, SP, BrazilDepartment of Clinical Analysis, Toxicology and Food Science, Faculty of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, 14040-903 Ribeirão Preto, SP, BrazilDepartament of Chemistry, Faculty of Philosophy, Sciences and Letters of Ribeirão Preto, University of São Paulo, 14040-901 Ribeirão Preto, SP, BrazilDepartment of Pharmaceutical Sciences, Faculty of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, 14040-903 Ribeirão Preto, SP, BrazilLevetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.http://dx.doi.org/10.1155/2016/5976324
spellingShingle Greyce Kelly Steinhorst Alcantara
Leandro Augusto Calixto
Luiz Alberto Beraldo de Moraes
Regina Helena Costa Queiroz
Anderson Rodrigo Moraes de Oliveira
Cristiane Masetto de Gaitani
Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
Journal of Analytical Methods in Chemistry
title Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
title_full Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
title_fullStr Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
title_full_unstemmed Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
title_short Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry
title_sort determination of levetiracetam in human plasma by dispersive liquid liquid microextraction followed by gas chromatography mass spectrometry
url http://dx.doi.org/10.1155/2016/5976324
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