Acidic metabolite profiling analysis of catecholamine and serotonin as O-ethoxycarbonyl/tert-butyldimethylsilyl derivatives by gas chromatography-mass spectrometry.
A novel derivatization method was developed for the simultaneous determination of six acidic metabolites of catecholamine and serotonin by gas chromatography-mass spectrometry (GC-MS). The metabolites were converted to O-ethoxycarbonyl/tert-butyldimethylsilyl (EOC/TBDMS) derivatives for the direct GC-MS analysis in selected ion monitoring mode. Their mass spectral pattern as EOC/TBDMS derivatives showed characteristic fragment ions of [M - 15](+) and [M - 57](+), which permitted rapid and accurate structural confirmation of acidic metabolites. The present method was linear (r ≥ 0.998), reproducible (percentage relative standard deviation = 1.0-10.0) and accurate (% relative error = -9.7-9.8) with detection limits of 0.001-4.7 ng/mL. When applied to human urine samples, the method allowed simultaneous determination of six acidic metabolites of catecholamine and serotonin.
Department of Molecular Science and Technology, Ajou University, Suwon, Republic of Korea.
Duc-Toan
DT
Nguyen
In-Seon
IS
Cho
Jeong-Whun
JW
Kim
Kyoung-Rae
KR
Kim
Gwang
G
Lee
Man-Jeong
MJ
Paik
D000328:Adult; D001669:Biochemical Phenomena; D002395:Catecholamines / Q000737:chemistry / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D017646:Organosilicon Compounds / Q000737:chemistry*; D015203:Reproducibility of Results; D012701:Serotonin / Q000737:chemistry / Q000652:urine*; D012821:Silanes
D002395:Catecholamines; D017646:Organosilicon Compounds; D012821:Silanes; C009660:t-butyldimethylsilyl compounds; C103256:tert-butyldimethylsilane; D012701:Serotonin