Article ID Journal Published Year Pages File Type
1213030 Journal of Chromatography B 2013 10 Pages PDF
Abstract

•A GC/MS/MS method was proposed for the profiling analysis of bioamines and metabolites in brain tissue.•Selective derivatization and MCX-SPE were shown to have good performance for the target analysis by GC/MS.•MRM mode provided high sensitivity and specificity for the targets in brain tissue.•The developed method was validated in terms of linearity, LLOD, LLOQ, precision and accuracy.•The LLOQs of the target analytes were at least 10 fold lower than those from GC/MS-SIM.

The profiling analysis of biogenic amines, including catecholamines and serotonin, and their metabolites in mouse brain tissue provides an important key to understanding their roles in the body and the possibility of simple and accurate diagnosis of neural diseases. A novel approach in the analysis of biogenic amines and their acidic metabolites in brain tissue using gas chromatography–tandem mass spectrometry (GC–MS/MS) is presented. Biogenic amines and their acidic metabolites in brain tissue were effectively separated using a mixed-cation-exchange solid-phase extraction (MCX-SPE) cartridge with a variation in the composition of the SPE elution solvents. A selective derivatization with hexamethyldisilazane (HMDS) and N-methyl-bis-heptafluorobutyramide (MBHFBA) was used to increase the detection sensitivity and to prevent the formation of any side-products. The identification and quantification of the target analytes were performed by gas chromatography triple quadrupole mass spectrometry (GC–MS/MS) using multiple ion reaction monitoring (MRM) mode. The overall recovery yields of the biogenic amines and their metabolites were above 87.5% at 10 ng/g and 92.4% at 100 ng/g of spiking concentration range. The isotopic-labeled internal standards were used for the precise quantification of bioamines and their metabolites. The calibration curves for the biogenic amines and their metabolites obtained through GC–MS/MS were linear (r2 > 0.995) over the concentration range of 1 (2 or 3)–200 ng/mL. The present method was reproducible (relative standard deviation range 0.6–9.3%) and accurate (range 85.4–107.9%), with LLOQs of 0.71–3.69 ng/mL. The developed method was successfully applied to the determination and quantification of bioamines and their metabolites in rat brain tissue samples.

Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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