【摘要】 利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-乙醇(BCE)作为柱前衍生化试剂,在Eclipse XDB-C8色谱柱上,通过梯度洗脱对19种游离脂肪酸进行了分离和在线质谱定性.以乙腈为溶剂,1-乙基-3-(3-二甲氨基丙基)环己碳二亚胺(EDAC)作为缩合剂,4-二甲氨基吡啶为碱催化剂(DMAP),60℃下衍生反应40 min后获得稳定的荧光产物.激发和发射波长分别为eλx=333 nm,λem=390 nm.采用大气压化学电离源(APCI)正离子模式,实现了土壤中脂肪酸的定性及相应含量测定.脂肪酸的线性回归系数大于0.9993,检测限在11.79-33.04 fmol.更多还原

【Abstract】 A simple and highly sensitive method based on the derivatization of fatty acids utilizing 1,2-benzo-3,4-dihydrocarbazole-9-ethanol(BCE) as the novel precolumn derivatization reagent followed by high-performance liquid chromatography with fluorescence detection and online mass spectrometric identification is developed.Derivatization is obtained by the reaction of fatty acids with BCE at 60℃ for 40min in the presence of EDAC and DMAP in acetonitrile solvent.Derivatives are sufficiently stable to be efficiently analyzed by high-performance chromatography without pre-treatment.On a reversed-phase XDB-C8 column,nineteen kinds of free fatty acids(C1-C19) derivatives are separated and are sepctrometric identified online in conjunction with a gradient elution.The precise determination of fatty acids from soil sample is achieved by post-column online mass spectrometric identification with atmospheric pressure chemical ionization(APIC) source under positive mode detection.Linear responses are observed with coefficients of >0.9992,detection limits(at signal-to-noise of 3∶1) are 11.7933.04 fmol.更多还原