Jalilian Niloofar, Ebrahimzadeh Homeira, Asgharinezhad Ali Akbar
Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
J Chromatogr A. 2017 May 26;1499:38-47. doi: 10.1016/j.chroma.2017.03.087. Epub 2017 Apr 2.
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.
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。