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Resolution of thyroxine hormone enantiomers by precolumn derivatization with a fluorescent chiral reagent using reversed-phase high performance liquid chromatography
Ist Teil von
Sepu, 2008-09, Vol.26 (5), p.559
Ort / Verlag
China
Erscheinungsjahr
2008
Link zum Volltext
Quelle
MEDLINE
Beschreibungen/Notizen
A highly fluorescent chiral tagging reagent, R(-)-4-(N,N-dimethylaminosulfonyl)-7-(3-isothiocy-anatopyrrolidino)-2,1,3-benzoxadiazole (R(-)-DBD-PyNCS), was employed for the enantiomer separation of thyroxine hormone, D,L-3,5,3',5'-tetraiodothyronine (T4) and L-3,5,3'-triiodothyronine (T3). The reaction of R(-)-DBD-PyNCS with the thyroxine enantiomers was carried out at 40 degrees C for 20 min under a basic medium surrounding to yield the corresponding pair of diastereomers. No racemization occurs during the tagging reaction under the optimized conditions. Various experimental parameters for the derivatization reaction including the concentration of tagging reagent, reaction temperature and reaction time have been studied in order to get the highest yield of T4/T3 derivatives. The structures of T4/T3 derivatives were identified based on high performance liquid chromatography-mass spectrometry (HPLC-MS) measurement in negative mode. The efficient separation of derivatives have been achieved by isocratic elution