丹酰氯柱前衍生仲胺的高效液相色谱-电化学检测方法的研究

A Research on the Determination of Trace Secondary Amines by Reversed Phase High Performance Liquid Chromatography with Electrochemical Detection

立了一种灵敏检测仲胺的新方法。首次以丹酰氯作为仲胺的电化学检测衍生试剂，对分离检测条件、仲胺的衍生条件及电化学定量检测条件作了详细的研究。以甲醇－２０ｍｍｏｌ／Ｌ的邻苯二甲酸氢钾缓冲液（７０∶３０，ｐＨ３．３）为淋洗液，采用安培检测器在Ｅ＝＋１．１Ｖ电压条件下，在ＰＥＲＫＩＮ－ＥＬＭＥＲ／ＨＳ－３Ｃ１８（８３ｍｍ×４．６ｍｍｉ．ｄ．，３μｍ）柱上实现了二甲胺、二乙胺和哌啶的良好反相分离和灵敏检测，线性范围超过两个数量级。二甲胺、二乙胺和哌啶的检出限分别为０．０２４，０．６０，０．０９０ｐｇ。７次测定结果的相对标准偏差分别为２．１％，３．５％，１．１％。

A new sensitive method for determination of ultratrace secondary amines has heen described. It is the first time to use dansyl chloride as electrochemical derivatization reagent for secondary amines. The optimum experimental conditions have heen established. At first, trace secondary amines were derivatised with dansyl chloride at 40℃ for 30 minutes, then the mixture was injected and separated on a PERKIN ELMER/HS 3 C18 (83mm×46mm i.d. 3μm) column with methanol aqueous solution (70/30,pH 33) which contained 20mmol/L potassium biphthalate buffer as mobile phase and detected with electrochemical detection at E=+11V(Ag/AgCl). The calibration curves were linear in the range of 0225 54pg for dimethylamine;11 264pg for diethylamine, 0.43 102pg for piperidine. The detection limits were 0024,060,0090pg respectively and the coefficients of variation were less than 35% (n=7).