Citation: CHEN Lin-Ji, ZHU Chao-Le, CAO Xiao-Ji, ZHOU Ting, YE Xue-Min, MO Wei-Min. Magnetic Solid Phase Extraction with Fe₃O₄-Grafted Nitrogen- Doped Graphene for Determination of Four Organochlorine Contaminants in Environmental Water Samples[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(5): 762-769. doi: 10.11895/j.issn.0253-3820.170016 shu

Magnetic Solid Phase Extraction with Fe₃O₄-Grafted Nitrogen- Doped Graphene for Determination of Four Organochlorine Contaminants in Environmental Water Samples

CHEN Lin-Ji ^1, ,
ZHU Chao-Le ¹ ,
CAO Xiao-Ji ^1,2 ,
ZHOU Ting ¹ ,
YE Xue-Min ² ,
MO Wei-Min ^1,2

1.
College of Chemical Engineering Science, Zhejiang University of Technology, Hangzhou 310014, China;
2.
Research Center of Analysis and Measurement, Zhejiang University of Technology, Hangzhou 310014, China

Received Date: 10 January 2017
Revised Date: 28 February 2017

Fe₃O₄-grafted nitrogen-doped graphene (Fe₃O₄/N-G) nanomaterials were synthesized by chemical co-precipitation method, and its adsorption properties were discussed preliminarily. It was demonstrated that the adsorption of parachlormetaxylenol on Fe₃O₄/N-G was not limited to uniform monolayer adsorption and the adsorption kinetic followed the pseudo-second-order kinetic mode. Then, an ultrasound-assisted magnetic solid-phase extraction with Fe₃O₄/N-G as the magnetic adsorbent has been developed for the determination of four compounds including triclosan, chloroxylenol, hexachlorobenzene and 2,2',4,4',5,5'-hexachlorobiphenyl in environmental water samples, in combination with gas chromatography coupled to tandem mass spectrometry. Several factors related to extraction efficiencies, such as the amount of adsorbent, extraction time, sample pH and desorption conditions were investigated. The proposed preparation procedure was as follows: 6.0 mg of Fe₃O₄/N-G was dispersed into 100 mL of water sample under ultrasound. After 15 s, the Fe₃O₄/N-G carrying four compounds was separated from the water sample by an external magnetic field. Then, the targets were eluted from Fe₃O₄/N-G with 3 mL of ethanol and 2 mL of dichloromethane, sequentially. Finally, the eluent was dried under a mild stream of nitrogen and reconstituted with methanol and dichloromethane (1∶1, V/V) for the subsequent GC-MS/MS analysis. Under the optimized condition, an excellent linearity was observed in the range of 0.1-10 ng/L for the four compounds, with the correlation coefficients ranging from 0.9983 to 0.9999. The limits of detections (S/N=3) ranged from 0.05 to 0.6 ng/L and the limits of quantity (S/N=10) ranged from 0.2 to 2.4 ng/L. The mean recoveries at three spiked levels ranged from 68.2% to 99.6%. The relative standard deviations (RSDs) of intraday and interday were in the range of 3.3%-6.9% and 3.4%-9.4% (n=6), respectively. The proposed method was demonstrated to be simple and feasible for the trace analysis of antimicrobial agents and organochlorine contaminants in environmental water samples.
- Nitrogen-doped graphene,
- Magnetic solid-phase extraction,
- Environmental water samples,
- Antimicrobial agents,
- Organochlorine contaminants
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通讯作者: 陈斌, bchen63@163.com

Magnetic Solid Phase Extraction with Fe₃O₄-Grafted Nitrogen- Doped Graphene for Determination of Four Organochlorine Contaminants in Environmental Water Samples