Analytical and Bioanalytical Chemistry

, Volume 411, Issue 10, pp 2239–2248 | Cite as

Magnetic stir cake sorptive extraction of trace tetracycline antibiotics in food samples: preparation of metal–organic framework-embedded polyHIPE monolithic composites, validation and application

  • Fuyou DuEmail author
  • Lingshun Sun
  • Wei Tan
  • Zongyu Wei
  • Honggang Nie
  • Zhujun Huang
  • Guihua RuanEmail author
  • Jianping Li
Research Paper


In this work, a novel Fe3O4@Cu3(btc)2-embedded polymerized high internal phase emulsion (Fe3O4@HKUST-1-polyHIPE) monolithic cake was synthesized, characterized and used as an adsorbent in the magnetic stir cake sorptive extraction (MSCSE) and determination of tetracycline antibiotics (TCs) in food samples by a combination of with high-performance liquid chromatography–fluorescence detection (HPLC-FLD). The prepared Fe3O4@HKUST-1-polyHIPE monolithic composites displayed a strong extraction ability and high column capacity due to enhanced interactions such as π–π interactions, hydrogen bonding, and electrostatic interactions. The extraction and desorption conditions were evaluated, and the calibration curves of four spiked TCs were linear (R2 ≥ 0.9991) in the range from 20 to 800 ng mL−1 for milk and egg samples, and 20 to 800 ng g−1 for chicken muscle and kidney samples. The limits of detection and the limits of quantification of the four TCs by using the proposed MSCSE-HPLC-FLD method were in the range of 1.9–4.6 and 5.5–13.9 ng mL−1 for milk and egg samples, and 1.8–3.7 and 5.3–13.0 ng g−1 for chicken muscle and kidney samples, respectively. The recoveries of the target TCs from spiked food samples were in the range from 86.6 to 110.7% with relative standard deviations lower than 7.0%. The proposed method was successfully applied for the determination of these four TCs in milk, egg, chicken muscle, and kidney samples.


Magnetic metal–organic framework Poly(high internal phase emulsion) Stir cake sorptive extraction Liquid chromatography–fluorescence detection Tetracycline antibiotics 


Funding information

This study was jointly supported by the National Natural Science Foundation of China (21465008 and 21665006), the Natural Science Foundation from Guangxi Zhuang Autonomous Region (2018GXNSFAA138134, 2015GXNSFAA139024, and 2015GXNSFFA139005), the project of High Level Innovation Team and Outstanding Scholar in Guangxi Colleges and Universities (Guijiaoren[2014]49), and the Research Program of Guangxi Specially-invited Experts (TingFa [2018] 39).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2019_1660_MOESM1_ESM.pdf (2.3 mb)
ESM 1 (PDF 2344 kb)


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Copyright information

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

Authors and Affiliations

  • Fuyou Du
    • 1
    • 2
    Email author
  • Lingshun Sun
    • 1
  • Wei Tan
    • 3
  • Zongyu Wei
    • 1
  • Honggang Nie
    • 4
  • Zhujun Huang
    • 1
  • Guihua Ruan
    • 1
    Email author
  • Jianping Li
    • 1
  1. 1.Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and BioengineeringGuilin University of TechnologyGuilinChina
  2. 2.Key Laboratory of Theoretical Organic Chemistry and Function Molecule of Ministry of Education, School of Chemistry and Chemical EngineeringHunan University of Science and TechnologyXiangtanChina
  3. 3.Department of Food and Chemical Engineering, Lushan College of GuangxiUniversity of Science and TechnologyLiuzhouChina
  4. 4.College of Chemistry and Molecular EngineeringPeking UniversityBeijingChina

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