摘要
通过水热合成法和溶胶凝胶法制备Fe3O4@NiSiO3磁性纳米粒子,该纳米粒子微球具有均一的形貌、良好的磁性和分散性。将合成的Fe3O4@NiSiO3磁性纳米粒子作为磁性固相萃取(MSPE)介质,并结合高效液相色谱(HPLC)建立了水样中痕量微囊藻毒素MC-LR的分析方法。在优化实验条件下,方法在0.25~146.5 μg/L浓度范围内呈良好的线性关系,相关系数(r)为0.999 1,检出限为0.011 μg/L。将该方法用于纯水中微囊藻毒素的分析,回收率为81.0%,对实际水样的回收率为66.7%~72.0%。表明Fe3O4@NiSiO3磁性纳米粒子具有良好的选择性富集能力,可用于水中痕量微囊藻毒素的萃取。
The Fe3O4@NiSiO3 magnetic nanoparticles(NPs) were prepared by hydrothermal synthesis and sol-gel method.The nanoparticles microspheres have uniform morphology,good magnetic properties and dispersion.In this study,the synthesized NPs as a magnetic solid phase extraction(MSPE) media were combined with high performence liquid chromatography(HPLC) to develop an effective method for the detection of trace microcystin-LR(MC-LR) in water samples.After optimizing the MSPE and HPLC chromatographic conditions,the method showed a good linear relationship in the range of 0.25-146.5 μg/L with correlation coefficient(r) of 0.999 1.The detection limit was 0.011 μg/L.The method was applied in the analysis of microcystin toxins in pure water sample and actual water samples with recoveries of 81.0% and 66.7%-72.0%,respectively.The results showed that Fe3O4 @NiSiO3 magnetic nanoparticles have good enrichment capability,and could be effectively used for the extraction of trace microcystin in water.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第9期1137-1141,共5页
Journal of Instrumental Analysis
基金
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)
关键词
磁性固相萃取
高效液相色谱
微囊藻毒素
磁性纳米粒子
magnetic solid-phase extraction(MSPE)
high performance liquid chromatography(HPLC)
microcystins(MCs)
magnetic nanoparticles