Park, Sun-Young Kang, Bo-Xin Quing-Li Kim, Hoon Sik Lee, Jungae Hong, Jongki 2024-01-20T21:03:22Z 2024-01-20T21:03:22Z 2021-09-03 2009-07-20 0253-2964 https://pubs.kist.re.kr/handle/201004/132308 GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in ail attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GUMS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide Sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration Curves based on the use of ail isotopically labeled internal standard show good linearity over the range assayed, 1 similar to 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs Studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment. English WILEY-V C H VERLAG GMBH PLASMA-FREE METANEPHRINE LIQUID-CHROMATOGRAPHY ISOTOPE-DILUTION VANILLYLMANDELIC ACID HOMOVANILLIC-ACID PHEOCHROMOCYTOMA NORMETANEPHRINE METABOLITES DIAGNOSIS URINE Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry Article 1 BULLETIN OF THE KOREAN CHEMICAL SOCIETY, v.30, no.7, pp.1497 - 1504 BULLETIN OF THE KOREAN CHEMICAL SOCIETY 30 7 1497 1504 scie scopus kci 000268554800015 2-s2.0-69249175066 Chemistry, Multidisciplinary Chemistry Article PLASMA-FREE METANEPHRINE LIQUID-CHROMATOGRAPHY ISOTOPE-DILUTION VANILLYLMANDELIC ACID HOMOVANILLIC-ACID PHEOCHROMOCYTOMA NORMETANEPHRINE METABOLITES DIAGNOSIS URINE Catecholamines Chemical derivatizations Mass fragmentation patterns GC/MS analsysis