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Position: Home > Articles > Pre-column Derivatization High Performance Liquid Chromatography with Fluorescence Detection-based Quantitation and Mass Spectrometric Identification of Aliphatic Amines FOOD SCIENCE 2009,30 (20) 406-410

脂肪胺化合物的HPLC荧光法测定及质谱鉴定

作  者：
刘素娟;尤进茂
单  位：
曲阜师范大学化学科学学院;牡丹江师范学院化学系
关键词：
高效液相色谱;荧光检测;柱前衍生;脂肪胺
摘  要：
采用合成的荧光试剂4-(1-甲基-1H-菲并[9,10-d]咪唑-2-)苯甲酸(MPIBA)对脂肪胺进行柱前衍生后,采用高效液相色谱(HPLC)分离和荧光检测。衍生物的荧光激发和发射波长分别为λex=260nm、λem=446nm。80℃条件下在四氢呋喃(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EclipseXDB-C8色谱柱(4.6×150mm,5μm)上,采用梯度洗脱对12种游离脂肪胺衍生物进行优化分离。采用大气压化学电离源(APCI)正离子模式进行在线柱后质谱定性,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10.5～53.4fmol范围内,对实际样品臭豆腐中脂肪胺的测定结果满意。
译  名：
Pre-column Derivatization High Performance Liquid Chromatography with Fluorescence Detection-based Quantitation and Mass Spectrometric Identification of Aliphatic Amines
作  者：
LIU Su-juan1,YOU Jin-mao2(1.Department of Chemistry, Mudanjiang Normal College, Mudanjiang 157012, China;2.College of Chemistry Science, Qufu Normal University, Qufu 273165, China)
关键词：
HPLC;fluorescence detection;pre-column derivatization;aliphatic amines
摘  要：
In order to determine aliphatic amines, a fluorescent material, 4-(1-methy-1H-phenanthro[9,10-d]imidazol-2-) benzoic acid(MPIBA), was synthesized through the derivatization of aliphatic amines at 80 ℃for 10 min in the presence of 1-ethyl-3(3-dimethylaminopropyl)-carbodiimide hydrochloride(EDC·HCl) catalyst in tetrahydrofuran solution.The maximum excitation and emission wavelengths of this stable derivative were 260 and 446 nm, respectively.The separation of these derivatized amines was achieved on a reversed-phase Eclipse XDB C8(4.6 × 150 mm i.d., 5μm) column using a gradient elution and exhibited a good baseline resolution.The identification of aliphatic amine derivatives was carried out by post-column online APCI/MS(atmospheric pressure chemical ionization) in a positive-ion mode.Excellent linear responses were observed with a coefficient of larger than 0.9996 and a detection limit(at signal-to-noise of 3:1) of 10.5-53.4 fmol.This established method provided satisfactory results for determining amines from bean curd with odor.

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