A method for determining valproic acid in human whole blood and urine via gas chromatography-mass spectrometry and small-scale inter-laboratory trial |
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| Affiliation: | 1. Department of Forensic Medicine, Graduate School of Biomedical and Health Sciences, Hiroshima University, Japan;2. Department of Legal Medicine, Nippon Medical School, Japan;3. Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Japan;4. Department of Food Sciences and Biotechnology, Graduate School of Science and Technology, Hiroshima Institute of Technology, Japan;5. Center for Cause of Death Investigation Research, Graduate School of Biomedical and Health Sciences, Hiroshima University, Japan;1. Forensic DNA Typing Laboratory, Centre of Excellence in Molecular Biology, University of the Punjab Lahore 53700, Pakistan;2. Faculty of Life Sciences and Informatics, Balochistan University of Information Technology, Engineering and Management Sciences, Quetta (BAUITEMS), Pakistan;1. Department of Forensic Medicine and Toxicology, All India Institute of Medical Sciences, Jodhpur 342005, India;2. School of Forensic Sciences, National Forensic Sciences University, Tripura 799001, India;3. Department of Diagnostic and Interventional Radiology, All India Institute of Medical Sciences, Jodhpur 342005, India;4. Department of Anatomy, All India Institute of Medical Sciences, Jodhpur 342005, India;5. Department of Anthropology, (UGC Centre of Advanced Study), Panjab University, Chandigarh 160014, India;1. Università degli Studi di Udine, Dipartimento di Area Medica, Medicina Legale, Italy;2. Azienda Sanitaria Friuli Occidentale (ASFO), Dipartimento di Prevenzione, SOSD di Medicina Legale, Italy;1. Institut Universitaire d’Anthropologie Médico-Légale, Faculté de Médecine, Université Côte d’Azur, 28 Avenue de Valombrose, 06107 Nice cedex 2, France;2. UMR E4320 TIRO-MATOs CEA/DRF/Institut Joliot, Université Nice Sophia-Antipolis, Université Côte d’Azur, Nice, France;3. CEPAM (UMR CNRS 7264), 24 avenue des Diables Bleus, 06300 Nice, France |
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| Abstract: | A simple and cost-effective method for analyzing valproic acid (VPA) in biological samples was developed. VPA was extracted in methyl tertiary-butyl ether (MTBE) and derivatized using trimethylsilyldiazomethane. The MTBE extract was analyzed by gas chromatography-mass spectrometry (GC-MS). The extraction recovery in human whole blood and urine was over 90 %, with good linearity in the range of 1.0 to 250 µg/mL of VPA. The RSD for 2.0, 20, and 200 μg/mL VPA in whole blood ranged from 0.9 to 4.7 % for intra-day and 1.5 to 5.9 % for inter-day. The RSD for 2.0, 20, and 200 μg/mL VPA in urine ranged from 1.9 to 2.6 % for intra-day and 1.2 to 2.9 % for inter-day. As a preliminary cross-validation study, a cross-check was conducted using blinded concentration samples. The results demonstrated that the assay data of the two laboratories were comparable. |
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| Keywords: | Valproic acid Trimethylsilyldiazomethane Whole blood Urine GC-MS |
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