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

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。

Solid-phase extraction based on mesoporous Fe 3 O 4@mSiO 2@Cu 2+magnetic nanoparticles coupled with high performance liquid chromatography for the determination of microcystins in water samples

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.