, Volume 81, Issue 2, pp 265–275 | Cite as

QuEChERS with Magnetic Hydrophilic–Lipophilic Balanced Adsorbent and Its Application in Multi-Class Veterinary Residues in Milk by Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hongcheng Liu
  • Tao Lin
  • Xin Lin
  • Jinliang Shao
  • Qiwan Li


Using magnetic hydrophilic–lipophilic balanced adsorbent (HLB), with divinylbenzene n-vinylpyrrolidone polymer as monomers and Fe3O4@C nanoparticles as magnetic material, a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method is proposed for veterinary residue analysis in milk. The magnetic Fe3O4@C-HLB adsorbent was fabricated via simple co-mixing method based on an “aggregate wrap” mechanism, which enabled magnetic solid-phase extraction. Thus, the resultant material can be separated from the solvent rapidly and conveniently by a magnet. The residues of regulatory interest in milk include β-lactams, aminoglyside, and macrolides. The analytes were quantified by ultra high-performance liquid chromatography coupled to an electrospray ionization tandem mass spectrometer operating in multiple reaction monitoring modes. The decision limit (CCα) was 0.1–0.8 µg/L, and the detection capability (CCβ) was 0.2–2 µg/L. The method was accurate with recoveries ranging from 70.5 to 98%. Good intra-precision and intermediate precision were obtained with RSD better than 10%.

Graphical Abstract


UHPLC–MS–MS Fe3O4@C-HLB adsorbent Multi-class veterinary residues 



This work was supported by Projection 2013RA012 (social development projection of Yunnan province), 2014DA001, 2015HC025 (talent plan and scientific innovation platform of Yunnan province).

Compliance with Ethical Standards

Conflict of interest

All Authors declare that we have no conflict of interest.

Ethical approval

This article does not contain any studies with human participants performed by any of the authors.


  1. 1.
    Yahaya N, Mitome T, Nishiyama N, Sanagi MM, Ibrahim WAW, Nur H (2013) J Pharm Innov 8(4):240–246CrossRefGoogle Scholar
  2. 2.
    Martínez-Huélamo M, Jiménez-Gámez E, Hermo MP, Barrón D, Barbosa J (2009) J Sep Sci 32:2385–2392CrossRefGoogle Scholar
  3. 3.
    Hermo MP, Nemutlu E, Kir S, Barrón D, Barbosa J (2008) Anal Chem Acta 613:98–105CrossRefGoogle Scholar
  4. 4.
    Christodoulou EA, Samanidou V (2007) J Sep Sci 30:2421–2429CrossRefGoogle Scholar
  5. 5.
    Kantiani L, Farré M, Sibum M, Postigo C, López de Alda M, Barceló D (2009) Anal Chem 81:4285–4292CrossRefGoogle Scholar
  6. 6.
    Han RW, Zheng N, Yu ZN, Wang J, Xu XM, Qu XY, Li SL, Zhang YD, Wang JQ (2015) Food Chem 181:119–126CrossRefGoogle Scholar
  7. 7.
    Zhan J, Yu XJ, Zhong YY, Zhang ZT, Cui XM, Peng JF, Feng R, Liu XT, Zhu Y (2012) J Chromatogr B 906:48–57CrossRefGoogle Scholar
  8. 8.
    Wang J, Leung D, Chow W, Chang J, Wong JW (2015) J Agric Food Chem 63(41):9175–9187CrossRefGoogle Scholar
  9. 9.
    Zhang Y, Li X, Liu X, Zhang J, Cao Y, Shi Z, Sun H (2015) J Dairy Sci 98(12):8433–8444CrossRefGoogle Scholar
  10. 10.
    Stubbings G, Bigwood T (2009) Anal Chim Acta 637:68–75CrossRefGoogle Scholar
  11. 11.
    Aguilera-Luiz MM, Vidal JLM, Romer-Gonzalez R (2008) J Chromatogr A 1205:10–18CrossRefGoogle Scholar
  12. 12.
    Socas-Rodríguez B, Lanková D, Urbancová K, Krtková V, Hernández-Borges J, Rodríguez-Delgado MÁ, Pulkrabová J, Hajšlová J (2017) Anal Bioanal Chem 409(18):4467–4477CrossRefGoogle Scholar
  13. 13.
    Zhou W, Ling Y, Liu T, Zhang Y, Li J, Li H, Wu W, Jiang S, Feng F, Yuan F, Zhang F (2017) J Chromatogr B 1061–1062:411–420CrossRefGoogle Scholar
  14. 14.
    Tuzimski T, Rejczak T (2017) J AOAC Int. Google Scholar
  15. 15.
    Rejczak T, Tuzimski T (2017) Food Chem 217:225–233CrossRefGoogle Scholar
  16. 16.
    Zhao PY, Wang L, Zhou L, Zhang FZ, Kang S, Pan CP (2012) J Chromatogr A 122:17–25CrossRefGoogle Scholar
  17. 17.
    Shen CY, Cao XW, Shen WJ, Jiang Y, Zhao ZY, Wu B, Yu KY, Liu H, Lian HZ (2011) Talanta 84:141–148CrossRefGoogle Scholar
  18. 18.
    Gilbert-Lopez B, Garcia-Reyes JF, Lozano A, Fernandez-Alba AR, Molina-Diaz A (2010) J Chromatogr A 1217:6022–6034CrossRefGoogle Scholar
  19. 19.
    Srivastava AK, Trivedi P, Srivastava MK, Lohani M, Srivastava LP (2011) Environ Monit Assess 176:465–473CrossRefGoogle Scholar
  20. 20.
    Correia-Sa L, Fernandes VC, Calhau C, Domingues VF, Delerue-Matos C (2013) Food Anal Methods 6:587–593CrossRefGoogle Scholar
  21. 21.
    Liu HC, Lin X, Lin T, Zhang YL, Luo YL, Li QW (2016) J Sep Sci 39:3594–3601CrossRefGoogle Scholar
  22. 22.
    Zhang XL, Niu HY, Pan YY, Shi YL, Cai YQ (2010) Anal Chem 82:2363–2371CrossRefGoogle Scholar
  23. 23.
    Sun L, Sun X, Du XB, Yue YS, Chen LG, Xu HY, Zeng QL, Wang H, Ding L (2010) Anal Chim Acta 665:185–192CrossRefGoogle Scholar
  24. 24.
    Ibarra IS, Rodriguez JA, Miranda JM, Vega M, Barrado E (2011) J Chromatograph A 1218:2196–2202CrossRefGoogle Scholar
  25. 25.
    Berrada H, Borrull F, Font G, Molto JC, Marce RM (2007) J Chromatogr A 1157:281–288CrossRefGoogle Scholar
  26. 26.
    Posyniak A, Zmudzki J, Mitrowska K (2005) J Chromatogr A 1087:259–264CrossRefGoogle Scholar
  27. 27.
    Romero-Gonzalez R, Lopez-Martinez JC, Gomez-Milan E, Garrido-Frenich A, Martinez-Vidal JL (2007) J Chromatogr B 857:142–148CrossRefGoogle Scholar
  28. 28.
    Kaufmann A, Butcher P, Maden K, Widmer M (2008) J Chromatogr A 1194:66–79CrossRefGoogle Scholar
  29. 29.
    Babin Y, Fortier S (2007) J AOAC Int 90:1418–1426Google Scholar
  30. 30.
    van Holthoon FL, Essers ML, Mulder PJ, Stead SL, Caldow M, Ashwin HM, Sharman M (2009) Anal Chim Acta 637:135–143CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany 2017

Authors and Affiliations

  • Hongcheng Liu
    • 1
    • 2
    • 3
  • Tao Lin
    • 1
    • 2
    • 3
  • Xin Lin
    • 1
    • 2
    • 3
  • Jinliang Shao
    • 1
    • 2
    • 3
  • Qiwan Li
    • 1
    • 2
    • 3
  1. 1.Supervision and Testing Center for Farm Product QualityMinistry of AgricultureKunmingPeople’s Republic of China
  2. 2.Laboratory of Quality and Safety Risk Assessment for Agro-ProductMinistry of AgricultureKunmingPeople’s Republic of China
  3. 3.Institute of Quality Standard and Testing TechnologyYunnan Academy of Agriculture ScienceKunmingPeople’s Republic of China

Personalised recommendations