Determination of fluoroquinolones in food samples by magnetic solid-phase extraction based on a magnetic molecular sieve nanocomposite prior to high-performance liquid chromatography and tandem mass spectrometry

  • Hao Yu
  • Yuqian Jia
  • Ri Wu
  • Xiangfeng ChenEmail author
  • T.-W. Dominic ChanEmail author
Research Paper


In this study, a magnetic molecular sieve material (Fe3O4@MCM-48) was synthesized by a combination of solvothermal and self-assembly methods. The physicochemical properties of the magnetic molecular sieve material were characterized by scanning electron microscopy, energy-dispersive spectroscopy, magnetic hysteresis loop measurements, transmission electron microscopy, powder X-ray diffraction, N2 adsorption–desorption analysis, and Fourier transform infrared spectroscopy. The as-synthesized nanocomposite showed various advantages, including easy magnetic-assisted separation, high specific surface area, and a highly interwoven and branched mesoporous structure. The Fe3O4@MCM-48 nanocomposite was then used as an effective adsorbent material for magnetic solid-phase extraction of fluoroquinolones (FQs) from water samples. The FQs in the extract were determined via liquid chromatography–tandem mass spectrometry. Adsorption and desorption factors that affected the extraction performance were systematically optimized using spiked purified water samples. Good linearity (with R2 > 0.99) was shown by this FQ detection system for FQ concentrations from 5 to 1000 ng L−1. Moreover, low detection limits (0.7–6.0 ng L−1) and quantitation limits (2.5–20.0 ng L−1) and satisfactory repeatability (relative standard deviation < 10%, n = 6) were achieved for water samples. The developed method was also validated for the analysis of FQs in meat and milk samples. Finally, FQs in food and drinking water samples were successfully determined using the developed method.

Graphical abstract


Fluoroquinolones Magnetic solid-phase extraction Food Tandem mass spectrometry Molecular sieve 



Financial support from the Natural Science Foundation of Shandong Province (ZR2017MB011), the Research Grant Council of the Hong Kong Special Administrative Region (Research Grant Direct Allocation refs. 3132667 & 4053152), and the Key R&D Program of Shandong Province (2017CXGC0223) are gratefully acknowledged.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest in regard to this work.

Supplementary material

216_2019_1726_MOESM1_ESM.pdf (574 kb)
ESM 1 (PDF 574 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Analysis and Test CentreQilu University of Technology (Shandong Academy of Sciences)JinanChina
  2. 2.Department of ChemistryThe Chinese University of Hong KongNew TerritoriesChina

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