氮杂多环光致发光分子用于食品中脂肪胺的分析及质谱鉴定  

Application of Nitrogen Heterocyclic Photoluminescence Molecule for the Determination of Aliphatic Amines in Food with HPLC and Identification with Atmospheric Pressure Chemical Ionization Mass Spectrometry

作　　者：刘凌君[1] 赵文臣[1] 索有瑞[2] 尤进茂[1,2] 

机构地区：[1]曲阜师范大学化学科学学院,生命有机分析重点实验室,山东曲阜273165 [2]中国科学院西北高原生物研究所,青海西宁810001

出　　处：《分析测试学报》2008年第9期942-946,950,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20075016)

摘　　要：对含氮类光致发光分子2-（11H-苯[a]咔唑）-异丙基氯甲酸酯进行柱前衍生处理，并经荧光检测对脂肪胺进行高效液相色谱（HPLC）分离和质谱定性。衍生物于λex=279nm产生强烈荧光，发射波长为λex=380nm。40℃下在pH9．0的硼酸缓冲液中，衍生反应3min后获得稳定的荧光产物。在Eclipse XDB-C8色谱柱（4．6mm×150mm，5μm）上，采用梯度洗脱对12种脂肪胺衍生物进行了优化分离。采用大气压化学电离源（APCI Source）正离子模式进行质谱定性，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复性，多数脂肪胺的线性回归系数大于0．9994，检出限在2．73～23．16fmol水平。A simple and highly sensitive method was developed for the determination of aliphatic amines（AA） in food using HPLC with fluorescence detection and identification with atmospheric pressure chemical ionization mass spectrometry （APCI MS）. It was based on the pre-column derivatization of aliphatic amine with a nitrogen heterocyclic photoluminescence molecule 2- （ 11H-benzo [ a ] carbazol-11-yl） isopropyl chloroformate （BCPC-Cl）. Stable amine derivatives were obtained in the presence of borate buffer（ pH 9.0） within 3 min. The maximum excitation and emission wavelengths were at 279 nm and 380 nm, respectively. Separation of 12 amine-derivatives was achieved by a gradient elution on a reversed-phase Eclipse XDB C8 （4.6 mm × 150 mm, 5 μm） column with a good baseline resolution. The identification of amine-derivatives was carried out by MS using APCI as the ion source in positive-ion mode. The relative standard deviation （RSD） of the retention time and the peak area were less than 0. 109% and 2. 671% , respectively. Good linear responses were observed with correlation coefficients r 〉 0. 999 4. The detection limits ranged from 2.73 to 23.16 fmol.

关 键 词：高效液相色谱-质谱 荧光检测 柱前衍生 脂肪胺 

分 类 号：O657.63[理学—分析化学] O623.73[理学—化学]