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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

Abstract

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

Keywords

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

Notes

Acknowledgements

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)

References

  1. 1.
    Gouvêa R, Santos FD, Aquino MD, Pereira VDA. Fluoroquinolones in industrial poultry production, bacterial resistance and food residues: a review. Rev Bras Cienc Avic. 2015;17:1–10.CrossRefGoogle Scholar
  2. 2.
    Riaz L, Mahmood T, Khalid A, Rashid A. Fluoroquinolones (FQs) in the environment: a review on their abundance, sorption and toxicity in soil. Chemosphere. 2018;191:704–20.CrossRefGoogle Scholar
  3. 3.
    Amorim CL, Maia AS, Mesquita RBR. Performance of aerobic granular sludge in a sequencing batch bioreactor exposed to ofloxacin, norfloxacin and ciprofloxacin. Water Res. 2014;50:101–13.CrossRefGoogle Scholar
  4. 4.
    Pan Z, Peng J, Chen Y, Zang X. Simultaneous determination of five fluoroquinolones by the selective high performance liquid chromatography associating with sensitive resonance light scattering and mechanism study. Microchem J. 2018;136:71–9.CrossRefGoogle Scholar
  5. 5.
    Urraca JL, Castellari M, Barrios CA, Moreno-Bondi MC. Multiresidue analysis of fluoroquinolone antimicrobials in chicken meat by molecularly imprinted solid-phase extraction and high performance liquid chromatography. J Chromatogr A. 2014;1343:1–9.CrossRefGoogle Scholar
  6. 6.
    Batt AL, Aga DS. Simultaneous analysis of multiple classes of antibiotics by ion trap LC/MS/MS for assessing surface water and groundwater contamination. Anal Chem. 2005;77:2940–7.CrossRefGoogle Scholar
  7. 7.
    Yang ZJ, Qin WD. Separation of fluoroquinolones in acidic buffer by capillary electrophoresis with contactless conductivity detection. J Chromatogr A. 2009;1216:5327–32.CrossRefGoogle Scholar
  8. 8.
    Sun X, Wang J, Li Y, Yang J, Jin J. Novel dummy molecularly imprinted polymers for matrix solid-phase dispersion extraction of eight fluoroquinolones from fish samples. J Chromatogr A. 2014;1359:1–7.CrossRefGoogle Scholar
  9. 9.
    Liu X, Wang XC, Tan F, Zhao HX, Quan X, Chen JW, et al. An electrochemically enhanced solid-phase microextraction approach based on molecularly imprinted polypyrrole/multi-walled carbon nanotubes composite coating for selective extraction of fluoroquinolones in aqueous samples. Anal Chim Acta. 2012;727:26–33.CrossRefGoogle Scholar
  10. 10.
    Wang Q, Wang Y, Zhang ZZ, Tong Y, Zhang L. Waxberry-like magnetic porous carbon composites prepared from a nickel-organic framework for solid-phase extraction of fluoroquinolones. Microchim Acta. 2017;184:4107–15.CrossRefGoogle Scholar
  11. 11.
    Fan WY, He M, Wu XR, Chen BB, Hu B. Graphene oxide/polyethyleneglycol composite coated stir bar for sorptive extraction of fluoroquinolones from chicken muscle and liver. J Chromatogr A. 2015;1418:36–44.CrossRefGoogle Scholar
  12. 12.
    Huo SH, Yan XP. Facile magnetization of metal-organic framework MIL-101 for magnetic solid-phase extraction of polycyclic aromatic hydrocarbons in environmental water samples. Analyst. 2012;137:3445–51.CrossRefGoogle Scholar
  13. 13.
    Gu ZY, Chen JQ, Jiang JQ, Yan XP. Metal-organic frameworks for efficient enrichment of peptides with simultaneous exclusion of proteins from complex biological samples. Chem Commun. 2011;47:4787–9.CrossRefGoogle Scholar
  14. 14.
    Herrera-Herrera AV, Ravelo-Pérez LM, Hernández-Borges J, Afonso MM, Palenzuela JA. Oxidized multi-walled carbon nanotubes for the dispersive solid-phase extraction of quinolone antibiotics from water samples using capillary electrophoresis and large volume sample stacking with polarity switching. J Chromatogr A. 2011;1218:5352–61.CrossRefGoogle Scholar
  15. 15.
    He X, Wang GN, Yang K, Liu HZ, Wu XJ. Magnetic graphene dispersive solid phase extraction combining high performance liquid chromatography for determination of fluoroquinolones in foods. Food Chem. 2017;221:1226–31.CrossRefGoogle Scholar
  16. 16.
    Rodríguez E, Navarro-Villoslada F, Benito-Peña E, Marazuela MD, Moreno-Bondi MC. Multiresidue determination of ultratrace levels of fluoroquinolone antimicrobials in drinking and aquaculture water samples by automated online molecularly imprinted solid phase extraction and liquid chromatography. Anal Chem. 2011;83:2046–55.CrossRefGoogle Scholar
  17. 17.
    Ibarra IS, Rodriguez JA, Páez-Hernández ME, Santos EM, Miranda JM. Determination of quinolones in milk samples using a combination of magnetic solid-phase extraction and capillary electrophoresis. Electrophoresis. 2012;33:2041–8.CrossRefGoogle Scholar
  18. 18.
    Anbia M, Khoshbooei S. Functionalized magnetic MCM-48 nanoporous silica by cyanuric chloride for removal of chlorophenol and bromophenol from aqueous media. JNSC. 2015;5:139–46.Google Scholar
  19. 19.
    Qiang ZM, Bao XL, Ben WW. MCM-48 modified magnetic mesoporous nanocomposite as an attractive adsorbent for the removal of sulfamethazine from water. Water Res. 2013;47:4107–41147.CrossRefGoogle Scholar
  20. 20.
    Mei M, Huang X. Determination of fluoroquinolones in environmental water and milk samples treated with stir cake sorptive extraction based on a boron-rich monolith. J Sep Sci. 2016;39:1908–18.CrossRefGoogle Scholar
  21. 21.
    Khodadoust S, Ghaedi M. Application of response surface methodology for determination of methyl red in water samples by spectrophotometry method. Spectrochim Acta A. 2014;133:87–92.CrossRefGoogle Scholar
  22. 22.
    Ferdig M, Kaleta A, Vo TDT, Buchberger W. Improved capillary electrophoretic separation of nine (fluoro)quinolones with fluorescence detection for biological and environmental samples. J Chromatogr A. 2004;1047:305–11.CrossRefGoogle Scholar
  23. 23.
    Jiménez-Lozano E, Marqués I, Barrón D, Beltrán JL, Barbosa J. Determination of pK a values of quinolones from mobility and spectroscopic data obtained by capillary electrophoresis and a diode array detector. Anal Chim Acta. 2002;464:37–45.CrossRefGoogle Scholar
  24. 24.
    Frenich AG, Romero-González R, Gómez-Pérez ML. Martinez Vidal JL. Multi-mycotoxin analysis in eggs using a QuEChERS-based extraction procedure and ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry. J Chromatogr A. 2011;1218:4349–56.CrossRefGoogle Scholar
  25. 25.
    Wang N, Wang YF, Omer AM, Ouyang XK. Fabrication of novel surface-imprinted magnetic grapheme oxide-grafted cellulose nanocrystals for selective extraction and fast adsorption of fluoroquinolones from water. Anal Bioanal Chem. 2017;409:6643–53.CrossRefGoogle Scholar
  26. 26.
    Su SC, Chang MH, Chang CL, Chang PC, Chou SS. Simultaneous determination of quinolones in livestock and marine products by high performance liquid chromatography. J Food Drug Anal. 2003;11:114–27.Google Scholar
  27. 27.
    Chen L, Zhang X, Xu Y, Du X, Sun X, Sun L, et al. Determination of fluoroquinolone antibiotics in environmental water samples based on magnetic molecularly imprinted polymer extraction followed by liquid chromatography-tandem mass spectrometry. Anal Chim Acta. 2010;662:31–8.CrossRefGoogle Scholar
  28. 28.
    Wu H, Shi Y, Guo X, Zhao S, Du J. Determination and removal of sulfonamides and quinolones from environmental water samples using magnetic adsorbents. J Sep Sci. 2016;39:4398–407.CrossRefGoogle Scholar
  29. 29.
    Liu C, Liao Y, Huang X. Preparation of a boronic acid functionalized magnetic adsorbent for sensitive analysis of fluoroquinolones in environmental water samples. Anal Methods. 2016;8:4744–54.CrossRefGoogle Scholar
  30. 30.
    Zheng HB, Mo JZ, Zhang Y, Gao Q, Ding J. Facile synthesis of magnetic molecularly imprinted polymers and its application in magnetic solid phase extraction for fluoroquinolones in milk samples. J Chromatogr A. 2014;1329:17–23.CrossRefGoogle Scholar
  31. 31.
    Jin T, Wu H, Gao N, Chen X, Lai H. Extraction of quinolones from milk samples using bentonite/magnetite nanoparticles before determination by high-performance liquid chromatography with fluorimetric detection. J Sep Sci. 2016;39:545–51.CrossRefGoogle Scholar
  32. 32.
    Kantiani L, Farré M, Barceló D. Rapid residue analysis of fluoroquinolones in raw bovine milk by online solid phase extraction followed by liquid chromatography coupled to tandem mass spectrometry. J Chromatogr A. 2000;1218:9019–27.CrossRefGoogle Scholar
  33. 33.
    Barreto F, Ribeiro CBD, Hoff RB, Costa TD. Development and validation of a high-throughput method for determination of nine fluoroquinolones residues in muscle of different animal species by liquid chromatography coupled to tandem mass spectrometry with low temperature clean up. J Chromatogr A. 2017;1521:131–9.CrossRefGoogle Scholar

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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