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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
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
【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0.1~15μg/L范围内呈现良好的线性,线性相关系数(r)为0.999 4,检出限为0.025μg/L,定量限为0.082μg/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。
【Abstract】 Mesoporousmagnetic nanoparticles of Fe3O4@mSiO2@Cu2+were synthesized by twomethods of hydrothermal synthesis and room temperature synthesis.The synthesizedmesoporous Fe3O4@mSiO2@Cu2+nanoparticles presented uniform sizes,goodmagnetic properties and specific selectivity.In this work,a novelmagnetic solid-phase extraction(MSPE)method based onmesoporous Fe3O4@mSiO2@Cu2+nanoparticles(NPs)coupled with high performance liquid chromatography(HPLC)was developed for the simultaneous extraction of trace amount ofmicrocystin-LR(MC-LR)in water samples.The MSPE extraction conditions and HPLC conditions were optimized.The results showed that good linear relationship(r = 0.999 4)was obtained between peak area andmass concentration of MC-LR in the range of 0.1-15μg/L.The limit of detection was 0.025 μg/L,and the limit of quantification was 0.082 μg/L.Furthermore,thismethod 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 ofmicrocystin-LR in water samples.
【Key words】 magnetic solid-phase extraction(MSPE); high performance liquid chromatogra-phy(HPLC); microcystins(MCs); water; magnetic nanoparticles; mesoporous;
- 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2015年05期
- 【分类号】O657.72;X832
- 【被引频次】16
- 【下载频次】431