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磁性固相萃取-液相色谱法测定环境水样中多种碱性染料 被引量:7

Determination of Basic Dyes in Environmental Water by Magnetic Solid Phase Extraction-High Performance Liquid Chromatography
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摘要 采用化学共沉淀法制备了Fe3O4磁性纳米材料(Fe3O4MNPs),通过X射线粉末衍射(XRD)和扫描电镜(SEM)对其进行了结构表征,结果表明,Fe3O4MNPs呈球状,大小均匀,平均直径小于50nm,具有良好顺磁性.使用十二烷基磺酸钠(SDS)修饰的方法,应用该磁性纳米材料成功吸附富集了环境水中多种碱性工业染料.通过分析pH、SDS质量浓度、Fe3O4MNPs和Fe3O4MNPs/SDS的Zeta电位对吸附能力的影响,推测吸附机理主要基于半胶束/胶束与碱性染料间的静电作用.以此为基础,建立了磁性固相萃取-高效液相色谱测定环境水样中的碱性嫩黄O、碱性橙21、碱性橙22和罗丹明B含量的分析方法,并对SDS加入量、溶液pH值、Fe3O4 MNPs质量浓度和解析溶剂进行了优化.在优化的条件下,富集因子超过100倍,4种染料在0.05—0.5mg/L范围内线性良好,相关系数尺均大于0.9997;加标回收实验测得4种染料的回收率为96.1%-108.7%,相对标准偏差(RSD)为1.08%~2.35%.方法操作简单,结果准确,重现性好,表明该纳米材料经SDS修饰后,在环境水中染料的吸附富集,检测预处理方面有着广泛的应用潜力. A Fe3O4 magnetic nanopartiele (Fe3O4 MNPs) was prepared by co-precipitating Fe^2+ and Fe^3+ ions in an ammonia solution. The Fe3O4 MNPs was charaeterized by X-ray diffraction (XRD) and scanning electron microscopy. The results show the Fe3O4 MNPs obtained possesses superparamagnetism and a good nano spherical particle with an average size of less than 50 nm. Coated by sodium dodecyl sulfonate (SDS) , the basic dyes were absorbed on the surface of Fe3O4 MNPs. Based on the effects of the pH of sample solution, the concentration of SDS, the Zeta potential of Fe3O4 MNPs and Fe3O4 MNPs/SDS on the absorption ability of Fe3O4 MNPs, the mechanism of absorption was speculated by the electrostatic effects between hemimicells/admicells and basic dyes. Magnetic solid-phase extraction method, based on SDS-coated Fe3O4 nanoparticles as a novel, simple, and fast pre-concentration method, was applied for pre-coneentration and fast isolation of four basic synthetic dyes in environment water prior to HPLC determination. The experimental parameters, including the pH value of sample solution, extraction times, elution solvent and volume, and elution time, were optimized. Under the optimized conditions, Fe3O4 nanoparticles were suecessfully used to extract basic dyes in the environmental water samples and the enrichment factor is 100-fold. The result showed that the method had good linearity ( r 〉 0. 999 7 ). Reeoveries obtained by analyzing the spiked water samples were in the range of 96. 1% - 108.7% and the relative standard deviations (RSDs) were between 1.08% and 2. 35%. The results indicated that the proposed method could be applied successfully for the determination of basic synthetic dyes in environmental water samples. The Fe3O4 MNPs coated by SDS can be used in the adsorption and sample-preparation of basic dyes in environmental water.
出处 《华南师范大学学报(自然科学版)》 CAS 北大核心 2015年第2期58-66,共9页 Journal of South China Normal University(Natural Science Edition)
基金 国家高技术研究发展计划(863计划)项目(2014AA022004) 国家自然科学基金项目(21275058) 广州市科学研究基金(2014J4100196)
关键词 磁性固相萃取 碱性染料 高效液相色谱 magnetic solid phase extraction basic dyes HPLC
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参考文献14

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