School of Materials and Chemical Engineering, Ningbo University of Technology, 201 Fenghua Road, Ningbo 315211, China.
Xiangshan Entry-Exit Inspection and Quarantine Bureau, Xiangshan 310014, China.
Talanta. 2018 Apr 1;180:254-259. doi: 10.1016/j.talanta.2017.12.059. Epub 2017 Dec 20.
In current study, a new polyethyleneimine (PEI)-modified attapulgite material was prepared serving as a solid support in matrix solid-phase dispersion for the extraction and determination (by atomic absorption spectrometry) of cadmium in seafood products. The major factors affecting PEI grafting were optimized using various PEI amounts and molecular weights. Parameters pivotal to MSPD extraction efficiency, like: pH, volume of eluting solvent, and the sorbent mass-to-sample ratio were investigated. Quantitative recoveries were achieved with 0.21g of fish sample, 0.13g of PEI-modified attapulgite dispersing agent, and 50% HNO eluting solution. The limit of detection and the limit of quantification were found to be 2.5 and 8.3μgkg for cadmium in surimi samples, respectively. The recoveries were in the range of 89.2-100.1%, with RSDs ranged from 3.0% to 7.9% (n = 5). When compared to the method stipulated by the Chinese National Standard GB 5009.15-2014, the newly developed MSPD provides comparable accuracy and even better repeatability for the analysis of the cadmium in real seafood samples.
在本研究中，制备了一种新型的聚乙烯亚胺（PEI）改性凹凸棒土材料，用作基质固相分散法中的固体支撑物，用于提取和测定（原子吸收光谱法）海产品中的镉。通过改变 PEI 的用量和分子量，优化了影响 PEI 接枝的主要因素。考察了影响 MSPD 萃取效率的参数，如：pH 值、洗脱溶剂体积和吸附剂质量与样品质量比。在鱼样质量为 0.21g、PEI 改性凹凸棒土分散剂质量为 0.13g、50%HNO3 洗脱溶液的条件下，可实现定量回收。在鱼糜样品中，镉的检出限和定量限分别为 2.5μgkg 和 8.3μgkg。回收率在 89.2%-100.1%之间，相对标准偏差（RSD）为 3.0%-7.9%（n=5）。与中国国家标准 GB 5009.15-2014 规定的方法相比，新开发的 MSPD 法用于分析实际海产品样品中的镉，具有相当的准确性，甚至更好的重复性。
