高效液相色谱-间接光度法同时检测己内酰胺副产物中1-磺酸环己烷羧酸及硫酸根离子  

Simultaneous determination of 1-sulfo-cyclohexane carboxylic acid and sulfate anion in the by-products of caprolactam by high performance liquid chromatographyindirect photometric analysis

作　　者：颜志祥[1] 段正康[1] 李立南[1] 李海涛[1] 陈秋云[1] 彭叶[1] 

机构地区：[1]湘潭大学化工学院绿色催化与反应工程国家重点实验室,湖南湘潭411105

出　　处：《色谱》2013年第2期174-178,共5页Chinese Journal of Chromatography

基　　金：湖南省高校创新平台开放基金项目(11k062)

摘　　要：提出了一种能够同时检测具有紫外吸收(UV)的有机物和无紫外吸收的无机物含量的强阴离子交换色谱法(IEC)。以检测己内酰胺副产物中的1-磺酸基环己烷羧酸(SCCA)粗盐为具体实例开展研究。强阴离子色谱柱以及UV检测器被用于同时分析SCCA和硫酸根离子。本实验基于高效液相色谱-间接光度检测法(HPLC-IPD)原理来测定SCCA和硫酸根离子,选用具有强紫外吸收能力的邻苯二甲酸作为本底试剂加入到流动相中产生信号。硫酸根离子和SCCA分别在0.10～10.0 g/L和0.50～40.0 g/L范围内呈良好的线性关系,相关系数分别为0.999 14和0.999 97;加标回收率分别为98.50%～101.00%和93.33%～97.40%,定量限均为0.10 g/L,符合色谱检测要求。该方法具有良好的分离选择性,可用于SCCA和硫酸根离子的同时检测。Abstract：quantification of 1-sulfo-cyclohexane carboxylic acid （SCCA） and sulfate anion in the by-products of caprolactam. An strong anion chromatographic column and an ultraviolet （UV） detector were chosen for the assay of SCCA and sulfate anion. Non-chromophore-containing sulfate anion is not directly adaptable to the commonly used ultraviolet detection of high per- formance liquid chromatography （ HPLC）. This paper reports the development and validation of an HPLC assay for SCCA and sulfate anion based on indirect ultraviolet detection. An ultravio- let-absorbing reagent （the probe）, phthalic acid （PA）, was added to the mobile phase to induce a signal for the compound. The proposed method was qualified based on the perform ance criteria of repeatability, intermediate precision and linearity. The limits of detection were I. 0 g/L for both the analytes. The linear ranges varied from 0.50 to 40.0 g/L for SCCA and from 0. 10 to 10.0 g/L for sulfate anion, with the correlation coefficients of 0. 999 97 and 0. 999 14, and the recoveries of 93.33% - 97.40% and 98.50% - 101.00%, respectively. The established method can be used in practice to determine SCCA and sulfate anion simultaneously with perfect separation selectivity.

关 键 词：阴离子交换色谱法 高效液相色谱 间接光度检测 硫酸根离子 1-磺酸基-环己烷羧酸 己内酰胺副产物 邻苯二甲酸 本底试剂 

分 类 号：O658[理学—分析化学]