Silver nanoparticle-cellulose composite for thin-film microextraction of Cd and Pb as dithiocarbamate derivatives followed by inductively-coupled plasma mass spectrometry determination

IF 5.2 Q1 CHEMISTRY, ANALYTICAL Advances in Sample Preparation Pub Date : 2022-10-01 DOI:10.1016/j.sampre.2022.100041
Inmaculada de la Calle, Diego Fernández-Rodríguez, Isela Lavilla, Carlos Bendicho
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引用次数: 2

Abstract

Preconcentration of Cd and Pb at ultratrace level in waters following filtration through silver nanoparticles-cellulose composites used for thin-film microextraction was performed. The new procedure was based on the formation of pyrrolidine dithiocarbamate (APDC) derivatives, which showed a large affinity toward the AgNPs. For this purpose, cellulose filters modified with AgNPs were prepared in situ upon reduction of silver ions by sodium tetrahydroborate. The effect of several experimental parameters such as the kind of derivatization agent and its concentration, sample pH, desorption conditions and volume of filtered sample was assessed. Cd and Pb were quantitated in the eluates by inductively coupled plasma-mass spectrometry (ICP-MS). Filters were characterized by scanning electron microscopy (SEM) in backscattering electron mode and combined with energy dispersive X-ray spectrometry, showing the presence of Ag and S in the cellulose filter. The repeatability expressed as relative standard deviation (RSD,%) was 1.4% for Cd and 5.8% for Pb. Methodological detection limits were 0.6 and 8.5 ng/L for Cd and Pb, respectively. The method was applied to several environmental waters.

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银纳米颗粒-纤维素复合薄膜微萃取镉和铅作为二硫代氨基甲酸酯衍生物,电感耦合等离子体质谱法测定
采用银纳米颗粒-纤维素复合材料进行薄膜微萃取,对水中镉和铅进行超痕量预富集。新方法是基于吡咯烷二硫代氨基甲酸酯(APDC)衍生物的形成,该衍生物对AgNPs具有很大的亲和力。为此,用四氢硼酸钠还原银离子,原位制备了用AgNPs修饰的纤维素过滤器。考察了衍生化剂种类及其浓度、样品pH、解吸条件和过滤后样品体积等实验参数的影响。采用电感耦合等离子体质谱法(ICP-MS)对洗脱液中的Cd和Pb进行定量分析。利用扫描电子显微镜(SEM)和能量色散x射线光谱对滤料进行了表征,结果表明纤维素滤料中存在Ag和S。重复性以相对标准偏差(RSD,%)表示,Cd为1.4%,Pb为5.8%。方法检出限分别为0.6和8.5 ng/L。将该方法应用于几种环境水体。
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