色谱

色谱 ›› 2018, Vol. 36 ›› Issue (5): 452-457.DOI: 10.3724/SP.J.1123.2017.11060

• 研究论文 • 上一篇    下一篇

悬浮固化分散液液微萃取-高效液相色谱法测定水体中邻苯二甲酸酯

吴翠琴1, 李颖1, 常淑萍1, 陈永亨1, 陈迪云1, 龚剑1, 许良智2   

  1. 1. 广州大学环境科学与工程学院, 珠江三角洲水质安全与保护教育部重点实验室, 广东省放射性核素污染 控制与资源化重点实验室, 广东 广州 510006;
    2. 四川大学华西第二医院妇产科, 四川 成都 610041
  • 收稿日期:2017-11-30 出版日期:2018-05-08 发布日期:2014-03-21
  • 通讯作者: 吴翠琴.Tel:15013072160,E-mail:wucuiqin@gzhu.edu.cn
  • 基金资助:

    国家自然科学基金项目（21207022，41473097，41673110）；广东省大学生创新训练项目（201611078039）；青-骨干教师出国研修项目（201709945007）.

Determination of phthalates in water by dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by high performance liquid chromatography

WU Cuiqin1, LI Ying1, CHANG Shuping1, CHEN Yongheng1, CHEN Diyun1, GONG Jian1, XU Liangzhi2   

  1. 1. School of Environmental Science and Engineering, Guangzhou University, Key Laboratory for Water Quality Security and Protection in Pearl River Delta of Ministry of Education, Guangdong Provincial Key Laboratory of Radio Nuclides Pollution Control and Resources, Guangzhou 510006, China;
    2. Department of Obstetrics and Gynecology, West China Second University Hospital, Sichuan University, Chengdu 610041, China
  • Received:2017-11-30 Online:2018-05-08 Published:2014-03-21
  • Supported by:

    National Natural Science Foundation of China (Nos. 21207022, 41473097, 41673110); Guangdong Provincial Undergraduate Innovative Training Program (No. 201611078039); Program of Study Abroad for Young Scholar (No. 201709945007).

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摘要：

建立了悬浮固化分散液液微萃取（SFO-DLLME）结合高效液相色谱（HPLC）快速测定水样中6种邻苯二甲酸酯（PAEs）的分析方法。通过对影响萃取效率因素的优化，确定了最佳萃取条件：十二烷醇萃取剂20 μL、萃取温度60℃、离子强度20 g/L、萃取时间1 min。6种PAEs在2~2000 μg/L范围内呈良好的线性关系，相关系数（r）为0.9995~0.9999，检出限（S/N=3）为0.3~0.6 μg/L。对自来水、湖水、江水、污水、海水、市售塑料瓶装纯净水和矿泉水进行测定，能检测到部分PAEs。对加标水样进行回收率试验（10、100和1000 μg/L），6种PAEs的回收率为84.9%~94.5%，相对标准偏差为4.1%~6.8%（n=5）。该法环保、简单，可用于实际水样中6种PAEs的检测分析。

关键词: 分散液液微萃取, 高效液相色谱, 邻苯二甲酸酯, 水样, 悬浮固化

Abstract: A rapid method for the determination of six phthalates (PAEs) in water samples was established by dispersive liquid-liquid microextraction (DLLME) based on solidification of floating organic drop (SFO) coupled with high performance liquid chromatography (HPLC). The influences of the SFO-DLLME parameters on extraction efficiencies were studied. Dodecanol (extraction solvent, 20 μL) was added to the water samples (containing 20 g/L NaCl) at 60℃, and the solution was shaken for 1 min. The results showed that the six PAEs were linear in the range of 2-2000 μg/L with correlation coefficients (r) between 0.9995 and 0.9999. The limits of detection (S/N=3) of the six PAEs ranged from 0.3 to 0.6 μg/L. The proposed method was applied to the analysis of the seven water samples obtained from different sources (tap water, lake water, river water, waste water, sea water, plastic bottled pure water and mineral water), and some PAEs were detected. The recoveries of the six PAEs in the spiked water samples were 84.9%-94.5%, and relative standard deviations were 4.1%-6.8% at three levels of 10, 100 and 1000 μg/L. The method is an environmentally friendly and convenient method for the routine analysis of the PAEs in water samples.

Key words: dispersive liquid-liquid microextraction (DLLME), high performance liquid chromatography (HPLC), phthalates (PAEs), solidification of floating organic drop (SFO), water samples

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