Citation: CAO Xiao-Ji, ZHOU Ting, XU Jia-Hui, CHAI Yun-Feng, YE Xue-Min. Magnetic Solid Phase Extraction Based on Ferroferric Oxide/Nitrogen-doped Graphene for Determination of Six Kinds of Carbonyl Compounds in Water Samples[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(3): 394-402. doi: 10.19756/j.issn.0253-3820.181653 shu

Magnetic Solid Phase Extraction Based on Ferroferric Oxide/Nitrogen-doped Graphene for Determination of Six Kinds of Carbonyl Compounds in Water Samples

1.
College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China;
2.
Research Center of Analysis and Measurement, Zhejiang University of Technology, Hangzhou 310014, China;
3.
Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China

Received Date: 17 October 2018
Revised Date: 27 December 2018

Fund Project: This work was supported by the Commonweal Technology Research Program of Zhejiang Province (Nos. 2017C33014, 2017C37008) and the National Natural Science Foundation of China (No.21602200).

In combination with 2,4-dinitrophenylhydrazine (DNPH) pre-column derivatization, an ultrasound-assisted magnetic solid phase extraction method with Fe₃O₄-grafted nitrogen-doped graphene (Fe₃O₄/N-G) nanomaterials as magnetic adsorbent was developed for the determination of acetone, acrolein, butenal, n-butanal, cyclohexanone and hexanal in environmental water samples by ultra performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). The derivation conditions were optimized by single-factor experiments as follows:the pH of water sample was adjusted to 3.0, and derivatization was performed for 40 min at 40℃ with 500 times of DNPH. As a result, the conversion ratios of 6 carbonyl compounds were in the range of 52.1%-86.6%. Several significant factors that affected the magnetic solid-phase extraction efficiency including the amount of magnetic nanoparticles, salt concentration and kinds of desorption solvent were also optimized using a response surface methodology. The optimal conditions were as follows:4.7 mg of Fe₃O₄/N-G was dispersed into 100 mL of water with ultrasonic extraction for 10 s. Then the adsorbents were separated by a magnet and eluted with 2 mL of acetonitrile. Finally, the eluent was dried under a mild stream of nitrogen gas and reconstituted with acetonitrile and water (1:1, V/V) for the subsequent UPLC-HRMS analysis. It was obvious that the excessive DNPH could be almost eliminated by the MPSE process. Under the optimal conditions, a good linearity was obtained in the concentration range of 2-100 ng/L, with correlation coefficients ranged from 0.9980 to 0.9995. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) ranged from 0.05 to 0.20 ng/L and 0.20 to 0.96 ng/L, respectively. The average recoveries at three spiked levels ranged from 74.1% to 101.0% with the inter-and intra-day precisions (n=6) of less than 6.3%. Moreover, the trace level of acetone, acrolein, butenal, n-butanal, and hexanal in real water samples has been successfully detected using the proposed method. Attributed to the excellent performances of Fe₃O₄/N-G, the proposed method was demonstrated to be simple, quick and high sensitive for the trace analysis of carbonyl compounds in water samples.
- Nitrogen-doped graphene,
- Magnetic solid-phase extraction,
- High resolution mass spectrometry,
- Carbonyl compounds
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