荧光衍生-高效液相色谱分离及质谱鉴定芳香胺  

Pre-column derivatization-HPLC determination of aromatic amines with fluorescence detection and mass spectral identification

作　　者：户宝军[1,2] 孙志伟[3] 高平 尤进茂[1,3] 

机构地区：[1]曲阜师范大学生命有机分析重点实验室,曲阜273165 [2]淄博市临淄区环保分局,淄博255400 [3]中国科学院西北高原生物研究所,西宁810001

出　　处：《分析试验室》2009年第2期34-37,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(20075016)项目资助

摘　　要：含氮杂环光致发光分子经柱前衍生化,采用荧光检测及柱后在线质谱鉴定对废水中胺类化合物进行了测定。衍生物荧光激发和发射波长分别为λex=275nm,λem=380nm。在pH8.0的硼酸钠缓冲液中,于40℃下衍生反应40min后获得稳定的荧光产物。在Hypersil BDS C18柱上,采用梯度洗脱对5种芳香胺衍生物进行了优化分离。采用大气压化学电离源(APCI Source)正离子模式进行在线的柱后质谱定性,实现了5种芳香胺衍生物的快速、准确测定。方法具有良好的重现性,线性回归系数大于0.9998,检出限在71～81fmol水平。A method for the detennination of aromatic amines in waste water using a nitrogen-containing photoluminescence molecule 2-（ 11H-benzo[a] carbazol-11-yl） isopropyl chlomformate （BCPC-C1） as a labeling reagent followed by pre-column derivatization-high performance liquid chromatography with fluorescence detection was developed. The sta-ble derivatives were obtained by the labeling reaction of BCPC-Cl with aromatic amines at 40 ℃ in the presence of borate buffer （pH 8.0） within 40 min. The maximum excitation and emission wavelengths were at λex = 275 nm, λem = 380 nm, respectively. Separation of 5 amine-derivatives was achieved by a gradient elution on a reversed-phase Hypersil BDS Cl8 （4.6 × 200 mm, 5 μm） column with a good baseline resolution. The identification of amine-derivatives was carried out by the online post-column MS using atmospheric pressure chemical ionization （APCI） as ion source in positive-ion detection mode. The established method exhibited excellent reproducibility and recovery. Excellent linear responses were observed with correlation coefficients above 0. 9998, and detection limits （at signal-to-noise of 3 ： 1 ） were 71 - 81 fmol levels.

关 键 词：高效液相色谱-质谱 荧光检测 柱前衍生 芳香胺 

分 类 号：O657.63[理学—分析化学]