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基于氨基双峰介孔二氧化硅纳米粒子的在线超声辅助分散微固相萃取用于人体生物样品中镉的预富集和测定

On-line Ultrasound-Assisted Dispersive Micro-Solid-Phase Extraction Based on Amino Bimodal Mesoporous Silica Nanoparticles for the Preconcentration and Determination of Cadmium in Human Biological Samples.

作者信息

Shirkhanloo H, Falahnejad M, Zavvar Mousavi H

机构信息

Occupational and Environmental Health Research Center (OEHRC), Iranian Petroleum Industry Health Research Institute (IPIHRI), Tehran, 1485733111, Iran.

Department of Chemistry, Semnan University, Semnan, Iran.

出版信息

Biol Trace Elem Res. 2016 Jun;171(2):472-481. doi: 10.1007/s12011-015-0538-6. Epub 2015 Oct 16.

DOI:10.1007/s12011-015-0538-6
PMID:26475301
Abstract

On-line ultrasound-assisted dispersive micro-solid-phase extraction (USA-DμSPE) has been developed for preconcentration and separation of trace amounts of Cd(II) ions in 0.5 mL of human biological samples. In a syringe with a nylon membrane, new synthetic bulky amino bimodal mesoporous silica nanoparticles (NH2-UVM7) were dispersed as a nanoadsorbent in 5 mL of diluted serum sample (1:10), and after ultrasonic shaking, the liquid phase was separated from the solid phase. At the optimized pH, the chemical and physical adsorption of cadmium ions occurred, respectively, based on complexation with amine groups of UVM7 (Cd:NH2-UVM7) and silica nanoparticles. The analyte was then back-extracted from the sorbent with nitric acid solution (0.2 M), and its concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). Under the optimized conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were obtained as 0.01-0.56 μg L(-1), 0.002 μg L(-1), and 25, respectively. The adsorption capacity of NH2-UVM7 was found to be 108.6 mg g(-1) of cadmium. The validation of the methodology was performed by the human standard reference material (HSRM).

摘要

在线超声辅助分散微固相萃取(USA-DμSPE)已被开发用于富集和分离0.5 mL人生物样品中的痕量镉(II)离子。在带有尼龙膜的注射器中,将新型合成的大体积氨基双峰介孔二氧化硅纳米颗粒(NH2-UVM7)作为纳米吸附剂分散在5 mL稀释血清样品(1:10)中,超声振荡后,将液相与固相分离。在优化的pH值下,镉离子分别基于与UVM7的胺基络合(Cd:NH2-UVM7)和二氧化硅纳米颗粒发生化学和物理吸附。然后用硝酸溶液(0.2 M)从吸附剂中反萃取分析物,并用电热原子吸收光谱法(ETAAS)测定其浓度。在优化条件下,线性范围、检测限(LOD)和富集因子(PF)分别为0.01-0.56 μg L(-1)、0.002 μg L(-1)和25。发现NH2-UVM7对镉的吸附容量为108.6 mg g(-1)。该方法通过人标准参考物质(HSRM)进行验证。

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