色谱 ›› 2016, Vol. 34 ›› Issue (10): 992-997.DOI: 10.3724/SP.J.1123.2016.06048

• 研究论文 • 上一篇    下一篇

响应面法优化萃取条件用于高效液相色谱分析饮用水中痕量邻苯二甲酸二(2-乙基己基)酯及其迁移规律

吴菲1,2, 吕晓丹1,2, 唐俊杰1,2, 陈绮娴1, 彭学堂1, 陈奇丹1,2   

  1. 1. 吉林大学珠海学院, 广东 珠海 519041;
    2. 珠海市吉林大学超分子材料研究所, 广东 珠海 519041
  • 收稿日期:2016-06-29 出版日期:2016-10-08 发布日期:2013-04-03
  • 通讯作者: 陈奇丹
  • 基金资助:

    国家自然科学基金项目(21307039);广东高校优秀青-创新人才培养计划项目(2013LYM_0120);广东省高等学校优秀青-教师培养计划(YQ2014231);广东省自然科学基金(2016A03031383).

Optimization of the extraction method for high performance liquid chromatography analysis of trace di(2-ethylhexyl)phthalate in drinking water by response surface methodology and the migration regularity

WU Fei1,2, LÜ Xiaodan1,2, TANG Junjie1,2, CHEN Qixian1, PENG Xuetang1, CHEN Qidan1,2   

  1. 1. Zhuhai College of Jilin University, Zhuhai 519041, China;
    2. Zhuhai Institute of Supramolecular Materials, Jilin University, Zhuhai 519041, China
  • Received:2016-06-29 Online:2016-10-08 Published:2013-04-03
  • Supported by:

    National Natural Science Foundation of China (No. 21307039); Foundation for Distinguished Young Talents in Higher Education of Guangdong China (No. 2013LYM_0120); Foundation for Distinguished Young Teachers in Higher Education of Guangdong China (No. YQ2014231); Natural Science Foundation of Guangdong China (No. 2016A03031383).

摘要:

应用响应面法辅助分析塑料瓶装饮用水中邻苯二甲酸二(2-乙基己基)酯(DEHP)的迁移,建立了一种快速、简便、环保的痕量塑化剂类污染物检测方法。在盐析作用下,使用正己烷涡旋萃取,经氮气浓缩后进行高效液相色谱-紫外检测。响应面最优分析法考察了盐量、涡旋时间和萃取液体积3个因素作为萃取条件对DEHP回收率的影响,得到最佳萃取条件:盐量为16 g/L、涡旋时间为90 s、萃取液体积为5.28 mL。在此实验条件下,DEHP的最大理论回收率为92.91%,实验验证值为92.97%,与理论值相差0.06%。本方法检出限为0.006 mg/L,满足中国国家标准规定的生活饮用水安全标准要求(0.008 mg/L),在0.01~15 mg/L范围内线性关系良好(相关系数R=0.9996)。选取常见市售饮用水样品进行分析,研究了塑料包装饮用水中痕量DEHP迁移的规律。与传统的优化方法相比,响应面模型分析法综合考虑了各因素的影响,而且更加简便、低成本、对环境友好,是实现样品中微痕量污染物精准检测的重要辅助手段。

关键词: 高效液相色谱, 邻苯二甲酸二(2-乙基己基)酯, 迁移规律, 响应面法, 饮用水

Abstract:

A simple and rapid method for the determination of trace di(2-ethylhexyl)phthalate (DEHP) in drinking water was developed and the migration regularity was studied. In this work, the migration of DEHP from plastic bottle products of supermarket was studied by high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV), and the extraction conditions were optimized by response surface methodology (RSM). With the effect of NaCl, DEHP in drinking water sample was extracted in n-hexane by vortex, dried and concentrated by N2, and then dissolved by methanol. The filtrate was injected into an HPLC-UV system for the analysis. The optimized extraction conditions were NaCl of 16 g/L, the vortex time of 90 s and the volume of n-hexane of 5.28 mL. Under the optimized conditions, the experimental value and the predicted value of the recoveries of DEHP were 92.97% and 92.91%, respectively, and the difference was only 0.063%. The limit of detection was 0.006 mg/L, the linear range was 0.01-15 mg/L (R=0.9996), and the relative standard deviation (RSD) was 0.015%-2.45%. In addition, the real water sample in plastic bottles from local supermarket was determined by the method and the migration regularity of trace DEHP in drinking water from plastic container under different temperature and time conditions was studied. The results showed that the application of RSM in the selection of optimal conditions for trace analysis is feasible, low-cost and eco-friendly.

Key words: di(2-ethylhexyl)phthalate (DEHP), drinking water, high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV), migration regularity, response surface methodology (RSM)

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