【摘要】 采用新型荧光试剂4-(1-甲基-1H-菲并[9,10-d]咪唑-2-)苯甲酸(MPIBA)进行柱前衍生并经荧光检测对脂肪胺进行了高效液相色谱(HPLC)分离.衍生物的荧光激发和发射波长分别为eλx=260 nm,eλm=446 nm.80℃下在四氢呋喃(THF)溶剂中用N-乙基-N-′[(3-二甲氨基)丙基]碳二亚胺盐酸盐(EDC)作催化剂,衍生反应10min后获得稳定的荧光产物.在Eclipse XDB-C8色谱柱(4.6×150 mm,5 mm)上,采用梯度洗脱对12种游离脂肪胺衍生物进行了优化分离,实现了各种脂肪胺衍生物的快速、准确测定.该方法具有良好的重现性,多数脂肪胺的线性回归系数大于0.9996,检测限在10.5-53.4 fmol范围内,对实际样品臭豆腐中脂肪胺的测定测定结果满意.更多还原

【Abstract】 A simple and sensitive method based on the derivatization of aliphatic amines with 4-(1-methy-1H-phenanthro[9,10-d]imidazol-2-)benzoic acid(MPIBA) followed by high-performance liquid chromatography(HPLC)with fluorescence detection and post-column mass spectrometric identification has been developed.The fluorescence excitation and emission wavelengths of derivatives are set at lex =260 and lem=446 nm,respectively.Optimal derivatization,giving the corresponding stable fluorescent derivatives,is obtained by the reaction of aliphatic amines with MPIBA at 80 ℃ for 10 min in the presence of 1-ethyl-3(3-dimethylaminopropyl)-carbodiimide hydrochloride(EDC.HCl) catalyst in acetonitrile.Separation of the derivatized amines in conjunction with a gradient elution is achieved on a reversed-phase Eclipse XDB C8(4.6×150 mm i.d.,5 mm) column with a good baseline resolution.Excellent linear responses are observed with coefficients >0.9996,detection limits(at signal-to-noise of 3∶1) are 10.5-53.4 fmol.The established method for the determination of amines from the extracted bean curd with odor exhibits satisfactory results.更多还原