Skip to main content
Log in

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction–high performance liquid chromatography–tandem mass spectrometry

  • Technical Note
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 μl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01–0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2

Similar content being viewed by others

References

  1. Hamscher G, Sczesny S, Höper H, Nau H (2002) Anal Chem 74:1509–1518

    Article  CAS  Google Scholar 

  2. Mueller SR, Singer H, Stoob K, Burkhardt M, Hartmann N, Goetz C, Stamm C, Waul C (2003) Mitt Lebensmittelunters Hyg 94:574–578

    CAS  Google Scholar 

  3. Christian T, Schneider RJ, Faerber HA, Skutlarek D, Goldbach HE, Meyer MT (2003) Acta Hydrochim Hydrobiol 31:36–44

    Article  CAS  Google Scholar 

  4. Schlüsener MP, Bester K, Spiteller M (2003) Anal Bioanal Chem 375:942–947

    Google Scholar 

  5. Martínez-Carballo E, González-Barreiro C, Scharf S, Gans O (2007) Environ Pollut 148:570–579

    Article  Google Scholar 

  6. Lindsey ME, Meyer M, Thurman EM (2001) Anal Chem 73:4640–4646

    Article  CAS  Google Scholar 

  7. Calamari D, Zuccato E, Castiglioni S, Bagnati R, Fanelli R (2003) Environ Sci Technol 37:1241–1248

    Article  CAS  Google Scholar 

  8. Seino A, Furusho S, Masunaga S (2004) J Jpn Soc Water Environ 27:685–691 (in Japanese)

    Article  CAS  Google Scholar 

  9. Hao C, Lissemore L, Nguyen B, Kleywegt S, Yang P, Solomon K (2006) Anal Bioanal Chem 384:505–513

    Article  CAS  Google Scholar 

  10. Kim S-C, Carlson K (2007) Anal Bioanal Chem 387:1301–1315

    Article  CAS  Google Scholar 

  11. Hirsch R, Ternes TA, Haberer K, Mehlich A, Ballwanz F, Kratz K-L (1998) J Chromatogr A 815:213–223

    Article  CAS  Google Scholar 

  12. Sacher F, Lange FT, Brauch H-J, Blankenhorn I (2001) J Chromatogr A 938:199–210

    Article  CAS  Google Scholar 

  13. Petrović M, Hernando MD, Diaz-Cruz MS, Barcelò D (2005) J Chromatogr A 1067:1–14

    Article  Google Scholar 

  14. Tang HP, Ho C, Lai SS (2006) Rapid Commun Mass Spectrom 20:2565–2572

    Article  CAS  Google Scholar 

  15. Stoob K, Singer HP, Goetz CW, Ruff, M, Mueller SR (2005) J Chromatogr A 1097:138–147

    Article  CAS  Google Scholar 

  16. Pozo OJ, Guerrero C, Sancho JV, Ibáñez M, Pitarch E, Hogendoorn E, Hernández F (2006) J Chromatogr A 1103:83–93

    Article  CAS  Google Scholar 

  17. Feitosa-Felizzola J, Temime B, Chiron S (2007) J Chromatogr A 1164:95–104

    Article  CAS  Google Scholar 

  18. Segura PA, Gagnon C, Sauv, é S (2007) Anal Chim Acta 604:147–157

    Article  CAS  Google Scholar 

  19. Tagiri-Endo M, Yanagita N (2007) Bunseki Kagaku 56:317–326 (in Japanese)

    Article  CAS  Google Scholar 

  20. Choi K-J, Kim S-G, Kim C-W, Kim S-H (2007) Chemosphere 66:977–984

    Article  CAS  Google Scholar 

  21. Loftin KA, Meyer MT, Adams CD, Surampalli R (2008) J Environ Qual 37:378–386

    Article  CAS  Google Scholar 

  22. Halling-Sørensen B, Lykkeberg A, Ingerslev F, Blackwell P, Tjørnelund J (2003) Chemosphere 50:1331–1342

    Article  Google Scholar 

  23. Khong S-P, Hammel Y-A, Guy PA (2005) Rapid Commun Mass Spectrom 19:493–502

    Article  CAS  Google Scholar 

  24. Bogialli S, Coradazzi C, Di Corcia A, Lagana A, Sergi M (2007) J AOAC Int 90:864–871

    CAS  Google Scholar 

  25. Xu J-Z, Ding T, Wu B, Yang W-Q, Zhang X-Y, Liu Y, Shen C-Y, Jiang Y (2008) J Chromatgr B 868:42–48

    Article  CAS  Google Scholar 

  26. Paesen J, Cypers W, Busson R, Roets E, Hoogmartens J (1995) J Chromatgr A 699:99–106

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Misako Tagiri-Endo.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Tagiri-Endo, M., Suzuki, S., Nakamura, T. et al. Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction–high performance liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 393, 1367–1375 (2009). https://doi.org/10.1007/s00216-008-2543-5

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-008-2543-5

Keywords

Navigation