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0.9994，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。
Mesoporous magnetic nanoparticles of Fe3O4@mSiO2@Cu2+ were synthesized by two methods of hydrothermal synthesis and room temperature synthesis. The synthesized meso-porous 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 perform-ance 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. 999 4) was obtained between peak area and mass 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,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.
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