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基于聚(1,8 - 二氨基萘)与磁性多壁碳纳米管复合材料制备的高效吸附剂的芳香胺分散微固相萃取

Dispersive micro-solid phase extraction of aromatic amines based on an efficient sorbent made from poly(1,8-diaminonaphtalen) and magnetic multiwalled carbon nanotubes composite.

作者信息

Jalilian Niloofar, Ebrahimzadeh Homeira, Asgharinezhad Ali Akbar

机构信息

Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.

Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.

出版信息

J Chromatogr A. 2017 May 26;1499:38-47. doi: 10.1016/j.chroma.2017.03.087. Epub 2017 Apr 2.

Abstract

In this work, the extraction of aromatic amines with an efficient magnetic multiwalled carbon nanotubes/FeO@Poly(1,8-diaminonaphtalen) (MWCNTs/FeO@PDAN) composite followed by HPLC-DAD was presented. Imprimis, the comparison among different magnetic nanosorbents including FeO, MWCNTs/FeO, FeO@PDAN and MWCNTs/FeO@PDAN was conducted. The obtained results, exhibited that the MWCNTs/FeO@PDAN composite has the highest extraction efficiency for target analytes (3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline). This sorbent was characterized by Fourier transform infrared spectroscopy, X-ray dispersive spectroscopy, thermogravimetry analysis, scanning electron microscopy, transition electron microscopy, vibrating sample magnetometry and X-ray diffraction. Design of experiment approach was applied to find out the optimal experimental conditions. The optimal extraction conditions were: pH of the sample, 10; sorbent amount, 10mg; sorption time, 15min; salt concentration, 10% w/w; type and volume of the eluent, 0.01molL HCl in acetonitrile, 145μL; elution time; 2min. Under the optimal extraction conditions detection limits and linear dynamic ranges were achieved in the range of 0.1-0.25μgL and 0.25-500μgL, respectively. The percent of extraction recovery and relative standard deviations (n=5) were in the range of 31.2-82.8% and 3.4-5.6%, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of target analytes in various water samples.

摘要

在本研究中,提出了一种利用高效磁性多壁碳纳米管/FeO@聚(1,8 - 二氨基萘)(MWCNTs/FeO@PDAN)复合材料萃取芳香胺,随后采用高效液相色谱 - 二极管阵列检测器(HPLC - DAD)进行分析的方法。首先,对包括FeO、MWCNTs/FeO、FeO@PDAN和MWCNTs/FeO@PDAN在内的不同磁性纳米吸附剂进行了比较。所得结果表明,MWCNTs/FeO@PDAN复合材料对目标分析物(3 - 硝基苯胺、4 - 氯苯胺、4 - 溴苯胺和3,4 - 二氯苯胺)具有最高的萃取效率。通过傅里叶变换红外光谱、X射线色散光谱、热重分析、扫描电子显微镜、透射电子显微镜、振动样品磁强计和X射线衍射对该吸附剂进行了表征。采用实验设计方法来确定最佳实验条件。最佳萃取条件为:样品pH值为10;吸附剂用量为10mg;吸附时间为15min;盐浓度为10% w/w;洗脱剂的类型和体积为乙腈中0.01mol/L HCl,145μL;洗脱时间为2min。在最佳萃取条件下,检测限和线性动态范围分别为0.1 - 0.25μg/L和0.25 - 500μg/L。萃取回收率和相对标准偏差(n = 5)分别在31.2 - 82.8%和3.4 - 5.6%范围内。最后,通过对各种水样中目标分析物的萃取和测定,成功证实了该方法的适用性。

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