A rapid and highly sensitive UPLC–MS/MS method using pre-column derivatization with 2-picolylamine for intravenous and percutaneous pharmacokinetics of valproic acid in rats
Autor: | Yang Hui Park, Jun Cheol Cho, Kyung Min Lim, Chang Geun Yi, Hye Jin Jeong, Dalwoong Choi, Kyung Mi Joo |
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Rok vydání: | 2013 |
Předmět: |
Male
Formic acid Administration Topical Clinical Biochemistry Tandem mass spectrometry Biochemistry Analytical Chemistry Rats Sprague-Dawley chemistry.chemical_compound Limit of Detection Tandem Mass Spectrometry Ammonium formate Animals Sample preparation Derivatization Chromatography High Pressure Liquid Detection limit Chromatography Valproic Acid Selected reaction monitoring Reproducibility of Results Cell Biology General Medicine Rats Standard curve Nonlinear Dynamics chemistry Administration Intravenous lipids (amino acids peptides and proteins) |
Zdroj: | Journal of Chromatography B. 938:35-42 |
ISSN: | 1570-0232 |
Popis: | A rapid, highly sensitive and specific ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) for the detection of valproic acid (VPA) in rat plasma following the topical application was developed and validated. This method was carried out with pre-column derivatization using 2-picolylamine (PA) which reacts with the carboxylic acid group of VPA. The derivatization was completed in 10min and the resulting PA-VPA derivative enabled the sensitive detection of VPA in selected reaction monitoring (SRM) mode. Sample preparation was done with simple liquid-liquid extraction and chromatographic separation was achieved within 5min on a C18 column using a gradient elution with the mobile phase of 2mM ammonium formate containing 0.1% formic acid and methanol. The standard curves were linear over the concentration range of 0.07-200μg/mL with a correlation coefficient higher than 0.99. The limit of detection (LOD) and the lower limit of quantification (LLOQ) was 0.03 and 0.07μg/mL, respectively with 100μL of plasma sample. The intra- and inter-day precisions were measured to be below 10.7% and accuracies were within the range of 94.1-115.9%. The validated method was successfully applied to the pharmacokinetics of VPA in the rat following topical and intravenous applications. |
Databáze: | OpenAIRE |
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