Chen Xiangming, Shi Yunwei, Zhao Xian'en, Zhang Haifeng, You Jinmao
College of Chemistry Science, Qufu Normal University, Qufu 273165, China.
Se Pu. 2005 Nov;23(6):642-5.
Aliphatic amines exist widely in nature. Therefore, quick and precise determination of aliphatic amines is of great significance. A simple and highly sensitive method based on the derivatization of aliphatic amines utilizing 1,2-benzo-3,4-dihydrocarbazole-9-acetic acid (BCAA) as the novel pre-column derivatization reagent followed by high performance liquid chromatography with fluorescence detection and online mass spectrometric identification was developed. Optimum derivatization was obtained by the reaction of aliphatic amines with BCAA at 50 degrees C for 15 min in the presence of 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDAC) in acetonitrile solvent. The condition of derivatization was mild and the yield of derivative each aliphatic amine was higher than 94%. Derivatives were sufficiently stable to be efficiently analyzed by high performance chromatography without pretreatment. On a reversed-phase BDS-C18 column, twelve aliphatic amine derivatives (C8 - C12) were separated under gradient elution with baseline resolution. The precise determining aliphatic amines from soil and wastewater samples was 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 coefficients over 0.999 3. The detection limits (at signal-to-noise ratio of 3: 1) were 12 - 28 fmol.
脂肪胺广泛存在于自然界中。因此,快速、准确地测定脂肪胺具有重要意义。本文建立了一种简单且高灵敏度的方法,该方法以1,2-苯并-3,4-二氢咔唑-9-乙酸(BCAA)作为新型柱前衍生试剂对脂肪胺进行衍生化,随后采用高效液相色谱-荧光检测及在线质谱鉴定。在乙腈溶剂中,脂肪胺与BCAA在50℃下于1-乙基-3-(3-二甲氨基丙基)碳二亚胺(EDAC)存在下反应15分钟,可获得最佳衍生化效果。衍生化条件温和,各脂肪胺衍生物的产率均高于94%。衍生物具有足够的稳定性,无需预处理即可通过高效液相色谱进行有效分析。在反相BDS-C18柱上,采用梯度洗脱实现了12种脂肪胺衍生物(C8 - C12)的基线分离。通过柱后在线质谱鉴定,采用大气压化学电离(APIC)源在正模式检测下,可对土壤和废水样品中的脂肪胺进行准确测定。所建立的方法具有出色的重现性和回收率。线性响应良好,相关系数超过0.999 3。检测限(信噪比为3:1时)为12 - 28飞摩尔。