色谱

色谱 ›› 2015, Vol. 33 ›› Issue (5): 449-454.DOI: 10.3724/SP.J.1123.2015.01009

• 特别策划：新型分离材料专栏 • 上一篇    下一篇

基于介孔Fe3O4@mSiO2@Cu2+磁性纳米粒子的固相萃取-高效液相色谱法测定水中微囊藻毒素

孙红1,2, 娄大伟1, 连丽丽1, 韩雪1,2, 郭亭秀1,3, 陈慧君1,2   

  1. 1. 吉林化工学院化学与制药工程学院, 吉林 吉林 132022;
    2. 吉林大学化学学院, 吉林 长春 130012;
    3. 东北师范大学化学学院, 吉林 长春 130024
  • 收稿日期:2015-01-09 出版日期:2015-05-08 发布日期:2015-04-23
  • 通讯作者: 娄大伟
  • 基金资助:

    国家自然科学基金项目(21375046);吉林省科技发展计划项目(20130521024JH,2013C041);吉林省教育厅"十二五"科学技术研究项目(2013313).

Solid-phase extraction based on mesoporous Fe3O4@mSiO2@Cu2+ magnetic nanoparticles coupled with high performance liquid chromatography for the determination of microcystins in water samples

SUN Hong1,2, LOU Dawei1, LIAN Lili1, HAN Xue1,2, GUO Tingxiu1,3, CHEN Huijun1,2   

  1. 1. College of Chemistry and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China;
    2. College of Chemistry, Jilin University, Changchun 130012, China;
    3. College of Chemistry, Northeast Normal University, Changchun 130024, China
  • Received:2015-01-09 Online:2015-05-08 Published:2015-04-23

PDF

181

摘要：

通过水热合成和常温合成的方法制备了介孔Fe3O4@mSiO2@Cu2+磁性复合纳米粒子(NPs),其具有均匀的尺寸大小、良好的磁性能和特异的选择性。本研究将合成的NPs用作磁性固相萃取(MSPE)介质,结合高效液相色谱(HPLC)发展了一种测定水样品中痕量微囊藻毒素MC-LR的方法。在优化MSPE和HPLC条件后,该方法在0.1~15 μg/L范围内呈现良好的线性,线性相关系数(r)为0.9994,检出限为0.025 μg/L,定量限为0.082 μg/L。进一步将该方法用于水样中痕量藻毒素分析,结果发现回收率达到78%。这一结果表明:制得的磁性纳米粒子具有良好的萃取性能,可有效用于水样中痕量藻毒素的测定。

关键词: 磁性固相萃取, 磁性纳米粒子, 高效液相色谱, 介孔, 水, 微囊藻毒素

Abstract:

Mesoporous magnetic nanoparticles of Fe3O4@mSiO2@Cu2+ were synthesized by two methods of hydrothermal synthesis and room temperature synthesis. The synthesized mesoporous Fe3O4@mSiO2@Cu2+ nanoparticles presented uniform sizes, good magnetic properties and specific selectivity. In this work, a novel magnetic solid-phase extraction (MSPE) method based on mesoporous Fe3O4@mSiO2@Cu2+ nanoparticles (NPs) coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction of trace amount of microcystin-LR (MC-LR) in water samples. The MSPE extraction conditions and HPLC conditions were optimized. The results showed that good linear relationship (r=0.9994) was obtained between peak area and mass concentration of MC-LR in the range of 0.1-15 μg/L. The limit of detection was 0.025 μg/L, and the limit of quantification was 0.082 μg/L. Furthermore, this method was used for the analysis of algal toxins in water samples with the recovery of 78%. The results indicated that Fe3O4@mSiO2@Cu2+ magnetic nanoparticles were good pretreatment alternatives for the concentration of microcystin-LR in water samples.

Key words: high performance liquid chromatography (HPLC), magnetic nanoparticles, magnetic solid-phase extraction (MSPE), mesoporous, microcystins (MCs), water

中图分类号: