Amiri Amirhassan, Saadati-Moshtaghin Hamid Reza, Zonoz Farokhzad Mohammadi, Targhoo Azadeh
Department of Chemistry, Faculty of Sciences, Hakim Sabzevari University, 9617976487 Sabzevar, Iran.
Department of Chemistry, Faculty of Sciences, Hakim Sabzevari University, 9617976487 Sabzevar, Iran.
J Chromatogr A. 2017 Feb 3;1483:64-70. doi: 10.1016/j.chroma.2016.12.083. Epub 2016 Dec 31.
In this work, aminopropyl modified silica-coated magnetite nanoparticles with Wells-Dawson heteropoly acid (PWFe@APSCMNPs) was first synthesized and underwent highly efficient magnetic solid-phase extraction (MSPE) of aromatic amines from aqueous samples. The resulted nanomaterials were characterized with different physicochemical techniques such as Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). Aniline, N,N-dimethylaniline, o-toluidine and 3-chloroaniline were selected as target compounds. The sample quantification was carried out using gas chromatography-flame ionization detector (GC-FID). Under optimal working conditions, the developed method showed good linearity (R>0.9912) in the range of 0.01-100ngmL. The method displays detection limits (at an S/N ration of 3) in the range from 0.003 to 0.01ngmL, and the limits of quantification (at an S/N ratio of 10) are between 0.01 and 0.04ngmL. The enrichment factors (EFs) were in the range of 75-113. Relative standard deviations (RSDs) are 4.8-8.3%. The applicability of the developed method was examined by analyzing different water samples (river water, tap water, well water and wastewater) and the relative recovery values for the spiked water samples were found to be in the range of 90.7-99.8%.
在本研究中，首次合成了负载Wells-Dawson杂多酸的氨丙基改性二氧化硅包覆磁铁矿纳米粒子（PWFe@APSCMNPs），并用于从水样中高效磁固相萃取芳香胺。通过傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）和振动样品磁强计（VSM）等不同的物理化学技术对所得纳米材料进行了表征。选择苯胺、N,N-二甲基苯胺、邻甲苯胺和3-氯苯胺作为目标化合物，采用气相色谱-火焰离子化检测器（GC-FID）进行样品定量分析。在最佳工作条件下，所建立的方法在0.01-100 ng/mL范围内具有良好的线性（R>0.9912）。该方法的检测限（信噪比为3）在0.003至0.01 ng/mL之间，定量限（信噪比为10）在0.01至0.04 ng/mL之间。富集因子（EFs）在75-113范围内，相对标准偏差（RSDs）为4.8-8.3%。通过分析不同水样（河水、自来水、井水和废水）考察了所建立方法的适用性，加标水样的相对回收率在90.7-99.8%范围内。
