Analysis of Sulfonamides in Animal Feeds by Liquid Chromatography with Fluorescence Detection

• Published in: Journal of agricultural and food chemistry Vol. 59; no. 10; pp. 5240 - 5247
• Main Authors: Borràs, Sílvia, Companyó, Ramon, Guiteras, Jacinto
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 25.05.2011
• Subjects: acetates; Analytical Methods; Animal Feed - analysis; Anti-Bacterial Agents - analysis; antibiotics; Biological and medical sciences; Chromatography, High Pressure Liquid - methods; derivatization; detection limit; Feed and pet food industries; feeds; fluorescence; fluorometry; Food Contamination - analysis; Food industries; Fundamental and applied biological sciences. Psychology; General aspects; high performance liquid chromatography; Methods of analysis, processing and quality control, regulation, standards; Spectrometry, Fluorescence; sulfonamides; Sulfonamides - analysis; Veterinary Drugs - analysis; liquid chromatography; sulfonamides; feed analysis; fluorescence detection; Kinetex; Analysis method; Sulfonamide; Animal; Fluorescence; Liquid chromatography; Control method; Detection; Feed
• ISSN: 0021-8561; 1520-5118
• DOI: 10.1021/jf2005595

Two analytical methodologies for the simultaneous analysis of eight sulfonamide antibiotics in animal feeds were developed. Analytes were extracted in a simple and rapid procedure by manual shaking with an ethyl acetate/ultrapure water mixture (99:1, v/v) without further sample cleanup. Mean recoveries ranging from 72.7% to 99.4% with relative standard deviations below 9% were achieved from spiked animal feed samples. Determination was carried out by high-performance liquid chromatography using fluorometric detection with precolumn derivatization. The separation of the derivatized compounds was performed using two different chromatographic columns: a conventional C18 column and a recently available core–shell particle Kinetex C18 column. Both methods were validated in-house in six different feed matrices, and the two approaches were compared. The experiments showed that the method using the Kinetex column was superior with regard to speed of analysis and precision, both under repeatability and intermediate reproducibility conditions. The limits of detection and quantification were also greatly improved, below 0.10 and 0.34 μg/g, respectively. Finally, this novel approach was successfully applied to the analysis of real feed samples.