A High Performance Liquid Chromatographic Method for the Determination of Nine Sulfonamides in Milk

  • Chapter
Analysis of Antibiotic/Drug Residues in Food Products of Animal Origin
  • 348 Accesses

Abstract

A High Performance Liquid Chromatographic (HPLC) method for the determination of sulfadiazine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethiazole, sulfamethazine, sulfachloropyridazine, sulfadimethoxine, and sulfaquinoxaline in milk is described. Milk (10mL) is extracted three times (50, 40, and 40mL) with chloroform/acetone, the extract evaporated to dryness, and redissolved in 5mL potassium phosphate buffer (1.0 molar, pH 4.4). Hexane (5mL) is added to extract the lipid materials. The aqueous buffer layer containing sulfonamides is passed through a cyclobond-I solid phase extraction (SPE) cartridge and the cartridge is washed with 5mL potassium phosphate buffer. The sulfonamides, which are retained on the cartridge, are then eluted with 4mL aqueous acetonitrile (20% water). The eluent is evaporated to remove acetonitrile and the final volume of the aqueous eluent is made to 4mL with ammonium acetate buffer. The eluent is analyzed by HPLC using a reverse phase column with UV detection at 265nm. The recoveries of individual sulfonamides ranged from 64.0% to 85.9% in samples fortified at 10 and 20ppb levels.

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

Access this chapter

Subscribe and save

Springer+ Basic
EUR 32.99 /Month
  • Get 10 units per month
  • Download Article/Chapter or Ebook
  • 1 Unit = 1 Article or 1 Chapter
  • Cancel anytime
Subscribe now

Buy Now

eBook
EUR 9.99
Price includes VAT (Germany)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
Softcover Book
EUR 53.49
Price includes VAT (Germany)
  • Compact, lightweight edition
  • Dispatched in 3 to 5 business days
  • Free ship** worldwide - see info
Hardcover Book
EUR 85.55
Price includes VAT (Germany)
  • Durable hardcover edition
  • Dispatched in 3 to 5 business days
  • Free ship** worldwide - see info

Tax calculation will be finalised at checkout

Purchases are for personal use only

Institutional subscriptions

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

Similar content being viewed by others

References

  1. Federal Register, 53 FR 9492, March 23, 1988, National Center for Toxicological Research Technical Report Experiment Number 418, March 1988, NCTR Jefferson, AR 72079.

    Google Scholar 

  2. A. R. Long, L. C. Hsieh, M. S. Malbrough, C. R. Short, and S. A. Barker, Multiresidue Method for the Determination of Sulfonamides in Pork Tissue, J. Agri. Food Chem., 38: 423 (1990).

    Article  CAS  Google Scholar 

  3. J. D. Weber and M. D. Smedley, Unpublished Milk Survey, Food and Drug Administration, Washington, DC (1988).

    Google Scholar 

  4. L. Larocque, G. Carignan, and S. Sved, Sulfamethazine(Sulfadimidine) Residues in Canadian Consumer Milk, J. Assoc. Off. Anal. Chem., 73: 365 (1990)

    PubMed  CAS  Google Scholar 

  5. Code of Federal Regulation, Title 21, 556. 640, 473 (1990).

    Google Scholar 

  6. D. E. Dixon-Holland, and S. E. Katz, Direct Competitive Enzyme Linked Immunosorbent Assay for Sulfamethazine (Sulfadimidine) Residues in Milk, J. Assoc. Off. Anal. Chem., 72: 447 (1989).

    PubMed  CAS  Google Scholar 

  7. A. F. Lott, R. Smither, and D. R. Vaughan, Antibiotic Identification by High Voltage Electrophoresis Bioautography, J. Assoc. Off. Anal. Chem., 68: 1018 (1985).

    PubMed  CAS  Google Scholar 

  8. C. W. Sigel, J. L. Woolley Jr., and C. A. Nichol, Specific TLC (thin layer chromatographic) Tissue Residue Determination of Sulfadiazine Following Fluorescamine Derivatization, J. Pharma. Sci., 64: 973 (1975).

    Article  CAS  Google Scholar 

  9. J. E. Roybal, S. B. Clark, J. A. Hurlbut, C. A. Geisler, R. J. Schmid, and S. L. Cross, A Rapid Thin Layer Chromatographic Screening Procedure for the Detection of Sulfamethazine in Milk, Laboratory Information Bulletin, 6: 3433 (1990).

    Google Scholar 

  10. S. B. Clark, R. G. Burkepile, S. L. Cross, J. M. Storey, J. E. Roybal, and C. A. Geisler, A Rapid Thin Layer Chromatographic Screening Procedure for the Detection of Eight Sulfomamides in Milk, Laboratory Information Bulletin, 7: 3528 (1991).

    Google Scholar 

  11. H. Holtmannspotter and H. P. Thier, Determination of Residues of Six Sulfonamides and Chloramphenicol by Gas Chromatography on Glass Capillary Columns, Dtsch. Lebensm. Rundsch. 78: 347 (1982).

    Google Scholar 

  12. M. A. Alawi and H. A. Ruessel, Determination of Sulphonamides in Milk by High Performance Liquid Chromatography with Electrochemical Detection, Fresenius’. Anal. Chem. 307: 382 (1981).

    Article  CAS  Google Scholar 

  13. R. Malisch, Multi-method for Determination of Residues of Chemotherapeutic and Antiparasitics and Growth Promoters in Foodstuffs of Animal Origin. I. General Procedure and Determination of Sulfonamides, Z. Lebensm. Unters. Forsch, 182: 385 (1986).

    Article  Google Scholar 

  14. M. M. L. Aerts, W. M. J. Beek, and V. A. T. Brinkman, Monitoring of Veterinary Drug Residues by a Combination of Continuous Flow Techniques and Column Switching High erformance Liquid Chromatography 1. Sulphonamides in Egg, Meat and Milk using Post Column Derivatization with Dimethylaminobenzaldehyde, J. Chromatography, 435: 97 (1988).

    Article  CAS  Google Scholar 

  15. J. D. Weber, and M. D. Smedley, Liquid Chromatographic Determination of Sulfamethazine in Milk, J. Assoc. Off. Anal. Chem.72: 445 (1989).

    PubMed  CAS  Google Scholar 

  16. M. D. Smedley and J. D. Weber, Liquid Chromatographic Determination of Multiple Sulfonamide Residues in Bovine Milk, J. Assoc. Off. Anal. Chem. 73: 875 (1990).

    PubMed  CAS  Google Scholar 

  17. M. Petz, High Pressure Liquid Chromatographic Determination of Residual Chloramphenicol, Furazolidone and Five Sulphonamides in Eggs, Meat and Milk, Z. Lebensm. Unters. Forsch., 176: 289 (1983).

    Article  CAS  Google Scholar 

  18. J. Unruh, E. Piotrowski, and D. P. Schwartz, Solid Phase Extraction of Sulfamethazine in Milk with Quantitation at Low ppb Levels Using Thin Layer Chromatography, J. Chromatography, 519: 179 (1990).

    Article  CAS  Google Scholar 

  19. A. R. Long, C. R. Short, and S. A. Barker, Method for Isolation and Liquid Chromatographic Determination of Eight Sulfonamides in Milk, J. Chromatography, 502: 87 (1990).

    Article  CAS  Google Scholar 

  20. V. K. Agarwal, Detection of Sulfamethazine Residues in Milk by High Performance Liquid Chromatography, J. Liauid Chromatograohv, 13: 3531 (1990).

    Article  CAS  Google Scholar 

  21. K. Uekama, F. Hirayama, M. Otagiri, M. Otagiri, Y. Otagiri, and K. Ikeda, Inclusion Complexation of B- Cyclodextrin With Some Sulfonamides in Aqueous Solution, Chem. Pharm. Bull, 26: 1162 (1978).

    Article  CAS  Google Scholar 

  22. V. K. Agarwal, Solid Phase Extraction of Sulfonamides Using Cyclobond-I Cartridges, J. Liauid Chromatography, 14: 699 (1991).

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Editor information

Editors and Affiliations

Rights and permissions

Reprints and permissions

Copyright information

© 1992 Springer Science+Business Media New York

About this chapter

Cite this chapter

Agarwal, V.K. (1992). A High Performance Liquid Chromatographic Method for the Determination of Nine Sulfonamides in Milk. In: Agarwal, V.K. (eds) Analysis of Antibiotic/Drug Residues in Food Products of Animal Origin. Springer, Boston, MA. https://doi.org/10.1007/978-1-4615-3356-6_13

Download citation

  • DOI: https://doi.org/10.1007/978-1-4615-3356-6_13

  • Publisher Name: Springer, Boston, MA

  • Print ISBN: 978-1-4613-6480-1

  • Online ISBN: 978-1-4615-3356-6

  • eBook Packages: Springer Book Archive

Publish with us

Policies and ethics

Navigation