摘要
采用荧光检测的方法对氯甲酸-9-芴甲酯柱前衍生的18种脂肪胺类化合物进行反相高效液相色谱分析。衍生物的荧光激发和发射波长分别为265nm和310nm。实验结果表明,通过向衍生体系中加入氨水的方法,可以有效地消除过量衍生试剂对分离的干扰。以乙胺为基准物质考察该方法的重复性。6次衍生产物保留时间和峰面积的相对标准偏差分别为0.57％和2.9％。此外,18种脂肪胺的浓度与峰面积呈较好的线性关系,检出限为29.3～56.4 nmol/L。对海水分析的结果表明该方法不受样品中盐的干扰,适合实际样品中脂肪胺类化合物的检测。
Using 9 - Fluorenylmethylchloroformate (FMOC - Cl) as pre - column derivatizing reagent, eighteen aliphatic amines are labelled and separated by means of RP - HPLC. The fluorescent derivatives could be detected with λex and λem respectively at 265 and 310 nm. In our experiments, ammonia is used for reacting with excessive FMOC - Cl to avoid disturbing the separation of derivatives and proved very effective. The method in conjunction with a gradient elution offers a good separation on a Hypersil BDS C18 column. With ethylamine as a testing compound, in 6 parallel derivatiza-tion, RSD values of the retention time and peak area are 0.57% and 2.9% . In addition, quite good linear relationship between the concentrations and peak areas of 18 aliphatic amines has been obtained and the detection limits range are from 29.3 nmol/L to 56.4 nmol/L. All these results demonstrate that the method proposed for derivatizatiorl and analysis of aliphatic amines is of good repeatibility, accurate quantitative capacity and high sensitivity. Further, This method has been successfully applied into the analysis of sea water, showing its potential in practical application.
出处
《现代仪器》
CAS
2004年第2期14-16,18,共4页
Modern Instruments
基金
十五攻关(色谱仪及专用部件的研制与开发)资助项目(No.G010101)
国家自然科学基金(No.20175029)
