Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection
Objective(s): Dispersive liquid-liquid microextraction coupled with gas chromatography (GC)-flame ionization detector was developed for the determination of valproic acid (VPA) in human plasma. Materials and Methods: Using a syringe, a mixture of suitable extraction solvent (40 µl chloroform) and dis...
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| Format: | Article |
| Language: | English |
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Mashhad University of Medical Sciences
2015-10-01
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| Series: | Iranian Journal of Basic Medical Sciences |
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| Online Access: | http://ijbms.mums.ac.ir/pdf_5461_44fb5fc8503cf8af6c63d6e3205be518.html |
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| author | Rana Fazeli-Bakhtiyari Vahid Panahi-Azar Mohammad Hossein Sorouraddin Abolghasem Jouyban |
| author_facet | Rana Fazeli-Bakhtiyari Vahid Panahi-Azar Mohammad Hossein Sorouraddin Abolghasem Jouyban |
| author_sort | Rana Fazeli-Bakhtiyari |
| collection | DOAJ |
| description | Objective(s): Dispersive liquid-liquid microextraction coupled with gas chromatography (GC)-flame ionization detector was developed for the determination of valproic acid (VPA) in human plasma.
Materials and Methods: Using a syringe, a mixture of suitable extraction solvent (40 µl chloroform) and disperser (1 ml acetone) was quickly added to 10 ml of diluted plasma sample containing VPA (pH, 1.0; concentration of NaCl, 4% (w/v)), resulting in a cloudy solution. After centrifugation (6000 rpm for 6 min), an aliquot (1 µl) of the sedimented organic phase was removed using a 1-µl GC microsyringe and injected into the GC system for analysis. One variable at a time optimization method was used to study various parameters affecting the extraction efficiency of target analyte. Then, the developed method was fully validated for its accuracy, precision, recovery, stability, and robustness.
Results: Under the optimum extraction conditions, good linearity range was obtained for the calibration graph, with correlation coefficient higher than 0.998. Limit of detection and lower limit of quantitation were 3.2 and 6 μg/ml, respectively. The relative standard deviations of intra and inter-day analysis of examined compound were less than 11.5%. The relative recoveries were found in the range of 97 to 107.5%. Finally, the validated method was successfully applied to the analysis of VPA in patient sample.
Conclusion: The presented method has acceptable levels of precision, accuracy and relative recovery and could be used for therapeutic drug monitoring of VPA in human plasma. |
| first_indexed | 2024-04-13T11:15:51Z |
| format | Article |
| id | doaj.art-a44193c19aec4ec3981586c2f5bdac18 |
| institution | Directory Open Access Journal |
| issn | 2008-3866 2008-3874 |
| language | English |
| last_indexed | 2024-04-13T11:15:51Z |
| publishDate | 2015-10-01 |
| publisher | Mashhad University of Medical Sciences |
| record_format | Article |
| series | Iranian Journal of Basic Medical Sciences |
| spelling | doaj.art-a44193c19aec4ec3981586c2f5bdac182022-12-22T02:48:58ZengMashhad University of Medical SciencesIranian Journal of Basic Medical Sciences2008-38662008-38742015-10-0118109799885461Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detectionRana Fazeli-Bakhtiyari0Vahid Panahi-Azar1Mohammad Hossein Sorouraddin2Abolghasem Jouyban3Liver and Gastrointestinal Diseases Research Center, Tabriz University of Medical Sciences, Tabriz, Iran|Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, IranDrug Applied Research Center, Tabriz University of Medical Sciences, Tabriz, IranDepartment of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, IranPharmaceutical Analysis Research Center and Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, IranObjective(s): Dispersive liquid-liquid microextraction coupled with gas chromatography (GC)-flame ionization detector was developed for the determination of valproic acid (VPA) in human plasma. Materials and Methods: Using a syringe, a mixture of suitable extraction solvent (40 µl chloroform) and disperser (1 ml acetone) was quickly added to 10 ml of diluted plasma sample containing VPA (pH, 1.0; concentration of NaCl, 4% (w/v)), resulting in a cloudy solution. After centrifugation (6000 rpm for 6 min), an aliquot (1 µl) of the sedimented organic phase was removed using a 1-µl GC microsyringe and injected into the GC system for analysis. One variable at a time optimization method was used to study various parameters affecting the extraction efficiency of target analyte. Then, the developed method was fully validated for its accuracy, precision, recovery, stability, and robustness. Results: Under the optimum extraction conditions, good linearity range was obtained for the calibration graph, with correlation coefficient higher than 0.998. Limit of detection and lower limit of quantitation were 3.2 and 6 μg/ml, respectively. The relative standard deviations of intra and inter-day analysis of examined compound were less than 11.5%. The relative recoveries were found in the range of 97 to 107.5%. Finally, the validated method was successfully applied to the analysis of VPA in patient sample. Conclusion: The presented method has acceptable levels of precision, accuracy and relative recovery and could be used for therapeutic drug monitoring of VPA in human plasma.http://ijbms.mums.ac.ir/pdf_5461_44fb5fc8503cf8af6c63d6e3205be518.htmlDispersive liquid-liquid-microextractionGas chromatography-flame- ionization detectorHuman plasmaValproic acid |
| spellingShingle | Rana Fazeli-Bakhtiyari Vahid Panahi-Azar Mohammad Hossein Sorouraddin Abolghasem Jouyban Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection Iranian Journal of Basic Medical Sciences Dispersive liquid-liquid-microextraction Gas chromatography-flame- ionization detector Human plasma Valproic acid |
| title | Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection |
| title_full | Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection |
| title_fullStr | Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection |
| title_full_unstemmed | Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection |
| title_short | Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection |
| title_sort | determination of valproic acid in human plasma using dispersive liquid liquid microextraction followed by gas chromatography flame ionization detection |
| topic | Dispersive liquid-liquid-microextraction Gas chromatography-flame- ionization detector Human plasma Valproic acid |
| url | http://ijbms.mums.ac.ir/pdf_5461_44fb5fc8503cf8af6c63d6e3205be518.html |
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