期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1401, 期 -, 页码 24-32出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2015.04.057
关键词
Meso-/macroporous; Magnetic solid phase extraction; Automated solid-phase extraction; Chlorobenzene; Carboxymethyl-beta-cyclodextrin; Matrix interference
资金
- National Natural Science Foundation of China [31070866]
- Natural Science Foundation of Zhejiang [Y15B050008, 2013C37033, LY13C200017, Pd2013088, 2013A610163]
- Science and Technology Project of Zhejiang and Ningbo [2014A610184, 2013A610241]
- State Administration of Grain [201313010]
- Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD)
- K.C. Wong Magna Fund of Ningbo University
A high-performance and selective adsorbent was developed for simultaneous extraction of 6 chlorobenzenes residues in soil samples by using magnetic solid phase extraction (MSPE) combined with automated SPE followed by gas chromatography-mass spectrometry (GC-MS). The adsorbent was synthesized by grafting carboxymethyl-beta-cyclodextrin (cm-beta-CD) on the surface of porous core-shell magnetic Fe3O4@flower like TiO2 microspheres (Fe3O4@fTiO(2)-CMCD), used as a carrier. The main factors (adsorbent amount, adsorption time, elution solvent, elution volume, and elution flow rate) affecting the extraction efficiency were investigated in detail. The adsorbent exhibited high loading capacity (25.6 mg g(-1) for 1,3-dichlorobenzene). This maybe due to meso-/macroporous TiO2 having high specific surface area; as a carrier of the beta-cyclodextrin film, it could obviously increase the number of recognition sites. The newly developed adsorbent also showed good selectivity towards chlorobenzenes based on host-guest interactions between beta-cyclodextrin (on adsorbent's surface) and targets, which can minimize complex matrix interference in soil samples. The proposed method was successfully applied for the analysis of environmental soil samples with recovery ranging from 87.3 to 104.3%. All target compounds showed good linearities with correlation coefficients (r) higher than 0.996. The limits of quantitation for the 6 CBs were 0.03-0.09 mu g kg(-1). These findings confirmed meso-/macroporous structure Fe3O4@fTiO(2)-CMCD as a highly effective extraction material for use in trace CB analyses in complex soil samples. (C) 2015 Elsevier B.V. All rights reserved.
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