高效液相色谱/间接紫外检测法分离测定脂肪胺  

Determination of Aliphatic Amines by High Performance Liquid Chromatography / Indirect Ultraviolet Detection

作　　者：卜文[1] 马亚杰[1] 于泓[1] 

机构地区：[1]哈尔滨师范大学化学化工学院,黑龙江哈尔滨150025

出　　处：《分析测试学报》2014年第2期203-207,共5页Journal of Instrumental Analysis

基　　金：黑龙江省教育厅科学技术研究项目(12531192)

摘　　要：建立了无紫外光吸收的脂肪胺的高效液相色谱/间接紫外检测分析方法.采用反相C18色谱柱,以对氨基苯酚盐酸盐-有机溶剂为流动相分离测定脂肪胺.研究了背景紫外吸收试剂、有机溶剂、对氨基苯酚盐酸盐对分离和测定的影响,并探讨了保留规律.结果表明,以0.5 mmol/L对氨基苯酚盐酸盐水溶液（pH4.0）-甲醇（80∶20）作为流动相,在柱温30℃、流速1.0 mL/min时,甲胺、乙胺和丙胺3种化合物在14min内完全分离,检出限分别为0.38、0.59、0.81 mg/L.将方法应用于环境水样的测定,加标回收率为97.8％ ～99.1％,相对标准偏差均不大于1.8％.A novel analytical method was developed for the determination of aliphatic amines （e· g.methylamine,ethylamine and propylamine） without ultraviolet absorption by high performance liquid chromatography-indirect ultraviolet detection.Chromatographic separation was performed on a reversed-phase C18 column using 4-aminophenol hydrochloride-organic solvent as mobile phase.Effects of the background ultraviolet absorption reagents,organic solvents and 4-aminophenol hydrochloride on separation and determination of aliphatie amines were investigated.The retention rules of aliphatic amines under different chromatographic conditions were formulated.The successful separation of three aliphatic amines was achieved in 14 min by using 0.5 mmol/L 4-aminophenol hydrochloride （pH 4.0）-methanol （80 ∶ 20） as mobile phase at a flow rate of 1.0 mL/min and a column temperature of 30 ℃.The detection limits of three aliphatic amines were 0.38,0.59,0.81 mg/L,respectively.The method was successfully applied in the determination of environmental water samples with recoveries of 97.8%-99.1% and relative standard deviations no more than 1.8%.The method was simple,accurate and reliable.

关 键 词：高效液相色谱法 脂肪胺 间接紫外检测 对氨基苯酚盐酸盐 

分 类 号：O657.72[理学—分析化学] O623.732[理学—化学]