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利用新型荧光试剂4-(1H-菲并[9,10-d]咪唑-2-)苯甲酸(PIBA)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)分离和在线质谱定性。激发和发射波长分别为ex=261nm,em=443nm。80℃下在吡啶溶剂中用N-乙基-N’-[(3-二甲氨基)丙基]碳二亚胺盐酸盐(EDC)做催化剂,衍生反应10min后获得稳定的荧光产物。在EclipseXDB-C8色谱柱(4.6150mm,5mm)上,梯度洗脱对12种游离脂肪胺衍生物进行了优化分离。采用大气压化学电离源(APCI)正离子模式,实现了各种脂肪胺衍生物的测定。多数脂肪胺的线性回归系数大于0.9999,检测限为10.5～53.4fmol。
Pre-column derivatization was carried out with a novel fluorescent reagent 4- (1H-phenanthro [9,10-d] imidazol-2-yl) benzoate (PIBA) and the fatty amine was separated by high performance liquid chromatography Qualitative online mass spectrometry. Excitation and emission wavelengths were ex = 261 nm, em = 443 nm, respectively. N-ethyl-N ’- [(3-dimethylamino) propyl] carbodiimide hydrochloride (EDC) was used as a catalyst in pyridine solvent at 80 ℃ for 10 min to obtain a stable fluorescent product. The 12 free aliphatic amine derivatives were optimally separated by gradient elution on an EclipseXDB-C8 column (4.6150 mm, 5 mm). The use of atmospheric pressure chemical ionization source (APCI) positive ion mode, to achieve a variety of fatty amine derivatives determination. The linear regression coefficients for most fatty amines were greater than 0.9999 with a detection limit of 10.5-53.4 fmol.