Santa T, Kimoto K, Fukushima T, Homma H, Imai K
Faculty of Pharmaceutical Sciences, University of Tokyo, Japan.
Biomed Chromatogr. 1996 Jul-Aug;10(4):183-5. doi: 10.1002/(SICI)1099-0801(199607)10:4<183::AID-BMC581>3.0.CO;2-I.
A new fluorescent reagent for carboxylic acids, 4-(N-hydrazinoformylmethyl-N-methyl)amino-7-N,N-dimethylaminosu lphonyl-2, 1,3-benzoxadiazole (DBD-CO-Hz) was synthesized and its applicability as a precolumn derivatization reagent in high-performance liquid chromatography (HPLC) was examined. DBD-CO-Hz reacted with saturated fatty acids in the presence of a condensing agent, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and pyridine at room temperature for 30 min to give fluorescent products. The reaction solution was subjected to a reversed-phase HPLC and detected fluorometrically at a wavelength of 550 nm with an excitation of 440 nm. The detection limits of the derivatives were at low fmol range on column.
合成了一种新型的羧酸荧光试剂4-(N-肼甲酰甲基-N-甲基)氨基-7-N,N-二甲基氨基磺酰基-2,1,3-苯并恶二唑(DBD-CO-Hz),并考察了其作为高效液相色谱(HPLC)柱前衍生试剂的适用性。DBD-CO-Hz在缩合剂1-乙基-3-(3-二甲基氨基丙基)碳二亚胺(EDC)和吡啶存在下,于室温与饱和脂肪酸反应30分钟,生成荧光产物。反应溶液进行反相HPLC分析,并在激发波长为440nm、检测波长为550nm处进行荧光检测。衍生物的检测限在柱上为低飞摩尔范围。