Analytical and Bioanalytical Chemistry

, Volume 410, Issue 6, pp 1709–1724 | Cite as

Use of phenyl/tetrazolyl-functionalized magnetic microspheres and stable isotope labeled internal standards for significant reduction of matrix effect in determination of nine fluoroquinolones by liquid chromatography-quadrupole linear ion trap mass spectrometry

  • Fei Xu
  • Feng Liu
  • Chaozhan Wang
  • Yinmao Wei
Research Paper


In this study, the strategy of unique adsorbent combined with isotope labeled internal standards was used to significantly reduce the matrix effect for the enrichment and analysis of nine fluoroquinolones in a complex sample by liquid chromatography coupled to quadrupole linear ion trap mass spectrometry (LC-QqQLIT-MS/MS). The adsorbent was prepared conveniently by functionalizing Fe3O4@SiO2 microspheres with phenyl and tetrazolyl groups, which could adsorb fluoroquinolones selectively via hydrophobic, electrostatic, and π–π interactions. The established magnetic solid-phase extraction (MSPE) method as well as using stable isotope labeled internal standards in the next MS/MS detection was able to reduce the matrix effect significantly. In the process of LC-QqQLIT-MS/MS analysis, the precursor and product ions of the analytes were monitored quantitatively and qualitatively on a QTrap system equipped simultaneously with the multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan. Subsequently, the enrichment method combined with LC-QqQLIT-MS/MS demonstrated good analytical features in terms of linearity (7.5–100.0 ng mL-1, r > 0.9960), satisfactory recoveries (88.6%–118.3%) with RSDs < 12.0%, LODs = 0.5 μg kg-1 and LOQs = 1.5 μg kg-1 for all tested analytes. Finally, the developed MSPE-LC-QqQLIT-MS/MS method had been successfully applied to real pork samples for food-safety risk monitoring in Ningxia Province, China.

Graphical abstract

Mechanism of reducing matrix effect through the as-prepared adsorbent.


Magnetic solid-phase extraction Liquid chromatography-quadrupole linear ion trap mass spectrometry Fluoroquinolones Stable isotope labeled internal standards 



This work was supported by the National Natural Science Foundation of China (nos. 21475104, 21775121, and 21575114), the Industry Development Project by the Science and Technology Department of Shaanxi Province (no. 2016GY-214), and the Ningxia Provincial National Natural Science Foundation (no. NZ14226).

Compliance with Ethical Standards

Conflict of interest

The authors have declared no conflict of interest.

Supplementary material

216_2017_821_MOESM1_ESM.pdf (573 kb)
ESM 1 (PDF 572 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2017

Authors and Affiliations

  1. 1.Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials ScienceNorthwest UniversityXi’anChina
  2. 2.Ningxia Center for Disease Control and PreventionYinchuanChina

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