污水中脂肪胺荧光衍生物的高效液相色谱分离及质谱鉴定  

Determination of aliphatic amines in waste water by high performance liquid chromatography-mass spectrometry(HPLC/MS) with fluorescence detection

作　　者：陈向明[1] 董秀丽[1] 尤进茂[2] 

机构地区：[1]滨州医学院,烟台264003 [2]曲阜师范大学化学科学学院,曲阜273165

出　　处：《分析试验室》2009年第10期103-107,共5页Chinese Journal of Analysis Laboratory

摘　　要：利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-异丙基氯甲酸酯（BCIC）作为柱前衍生化试剂,在乙腈中,以硼酸钠缓冲液（pH 9）为催化剂,40℃下衍生反应10 min后获得稳定的荧光产物。在Eclipse XDB-C8色谱柱上,通过梯度洗脱对12种游离脂肪胺进行了分离和在线质谱定性。激发和发射波长分别为λex=333 nm,eλm=390 nm。采用大气压化学电离源（APCI）正离子模式,实现了污水中脂肪胺的定性及相应含量测定。脂肪胺的线性回归系数大于0.9996,检出限在10.57-37.83 fmol。Utilizing 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate（BCIC） as the novel pre-column fluorescence derivatization reagent,a simple and highly sensitive method to determinate aliphatic amines was developed.Optimum derivatization was obtained by the reaction of aliphatic amines with BCIC at 40 ℃ for 10min in the presence of sodium borate（pH 9） in acetonitrile solvent.Derivatives were sufficiently stable to be efficiently analyzed by high-performance liquid chromatography with fluorescence detection and online mass spectrometric identification. On a reversed-phase XDB-C8 column, twelve kinds of aliphatic amine （Cl - C12 ） derivatives were separated in conjunction with a gradient elution with a good baseline resolution. The precise determining aliphatic amines from wastewater sampies were obtained by post-column online mass spectrometric identification with atmospheric pressure chemical ionization （APIC） source under positive mode detection. The established method exhibited excellent reproducibility and recovery. Linear responses were observed with correlation coefficients larger than 0. 9996, the detection limits （at signal-to-noise of 3 ： 1） were 10.57 - 37.83 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：O657.7[理学—分析化学]