色谱

色谱 ›› 2013, Vol. 31 ›› Issue (2): 174-178.DOI: 10.3724/SP.J.1123.2012.09020

• 技术与应用 • 上一篇    

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

颜志祥, 段正康*, 李立南, 李海涛, 陈秋云, 彭叶   

  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
  • 收稿日期:2012-09-17 修回日期:2012-10-24 出版日期:2013-02-28 发布日期:2013-02-05
  • 通讯作者: 段正康
  • 基金资助:

    湖南省高校创新平台开放基金项目(11k062).

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

YAN Zhixiang, DUAN Zhengkang*, LI Linan, LI Haitao, CHEN Qiuyun, PENG Ye   

  1. State Key Laboratory of Green Catalysis and Reaction Engineering, College of Chemical Engineering, Xiangtan University, Xiangtan 411105, China
  • Received:2012-09-17 Revised:2012-10-24 Online:2013-02-28 Published:2013-02-05
  • Contact: Zhengkang Duan

PDF

497

被引次数

7

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0.99914和0.99997;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。

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

Abstract: An improved anion-exchange chromatographic method was developed for simultaneous 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 performance 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 ultraviolet-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 performance criteria of repeatability, intermediate precision and linearity. The limits of detection were 1.0 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 0.99997 and 0.99914, 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.

Key words: 1-sulfo-cyclohexane carboxylic acid, by-products of caprolactam, high performance liquid chromatography (HPLC), indirect photometric detection, phthalic acid, sulfate anion, the probe reagent, anion-exchange chromatography