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基于Fe@Ag@二巯基苯磁性固相萃取结合高效液相色谱法同时测定痕量镉、铅和汞离子

Simultaneous determination of cadmium, lead and mercury ions at trace level by magnetic solid phase extraction with Fe@Ag@Dimercaptobenzene coupled to high performance liquid chromatography.

作者信息

Zhou Qingxiang, Lei Man, Liu Yongli, Wu Yalin, Yuan Yongyong

机构信息

College of Geosciences, China University of Petroleum Beijing, Beijing 102249, China.

College of Geosciences, China University of Petroleum Beijing, Beijing 102249, China.

出版信息

Talanta. 2017 Dec 1;175:194-199. doi: 10.1016/j.talanta.2017.07.043. Epub 2017 Jul 14.

DOI:10.1016/j.talanta.2017.07.043
PMID:28841978
Abstract

Pollution resulted from heavy metal ions have absorbed much attention, and it is of great importance to develop sensitive and simultaneous determination method for them with common technologies without highly sensitive instruments. We prepared a new and functional core-shell magnetic nano-material, Fe@Ag@dimercaptobenzene (Fe@Ag@DMB), by a one-step method with sodium borohydride as the reducing agent and transmission electron microscopy (TEM) and energy dispersive spectrometer (EDS) were used for characterisation. The mercapto functional groups on the newly synthesised magnetic nanoparticles could interact with Cd, Pb, and Hg ions in water samples and then efficient extraction for Cd, Pb, and Hg ions was achieved. DDTC-Na solution was a good elutent for elution of these ions from Fe@Ag@DMB nanoparticles. Based on these, a sensitive method was developed for simultaneous preconcentration and determination of the aforementioned ions using magnetic Fe@Ag@DMB nanoparticles as the magnetic solid phase extraction adsorbent prior to high performance liquid chromatography coupled with variable wavelength detection. Under the optimal conditions, the detection limits of the three metal ions were in the range of 0.011-0.031μgL, and precisions were below 2.37% (n=6). The proposed method was evaluated with real water samples, and excellent spiked recoveries achieved indicated that the developed method would be a promising tool for monitoring these heavy metal ions in water samples.

摘要

由重金属离子导致的污染已备受关注,利用常规技术而非高灵敏度仪器开发对其进行灵敏且同时测定的方法具有重要意义。我们以硼氢化钠为还原剂,通过一步法制备了一种新型功能性核壳磁性纳米材料Fe@Ag@二巯基苯(Fe@Ag@DMB),并采用透射电子显微镜(TEM)和能量色散谱仪(EDS)进行表征。新合成的磁性纳米颗粒上的巯基官能团可与水样中的镉、铅和汞离子相互作用,进而实现对镉、铅和汞离子的高效萃取。二乙氨基二硫代甲酸钠(DDTC-Na)溶液是将这些离子从Fe@Ag@DMB纳米颗粒上洗脱下来的良好洗脱剂。基于此,开发了一种灵敏的方法,在高效液相色谱结合可变波长检测之前,使用磁性Fe@Ag@DMB纳米颗粒作为磁性固相萃取吸附剂,同时对上述离子进行预富集和测定。在最佳条件下,三种金属离子的检测限在0.011 - 0.031μg/L范围内,精密度低于2.37%(n = 6)。该方法用于实际水样的评估,获得的出色加标回收率表明所开发的方法将是监测水样中这些重金属离子的一种有前景的工具。

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