1. Magnetic solid phase extraction followed by high-performance liquid chromatography for the determination of sulphonamides in milk samples.
- Author
-
Ibarra IS, Miranda JM, Rodriguez JA, Nebot C, and Cepeda A
- Subjects
- Animals, Magnetic Phenomena, Sulfonamides analysis, Chromatography, High Pressure Liquid methods, Milk chemistry, Solid Phase Extraction methods, Sulfonamides chemistry
- Abstract
A simple and effective method based on magnetic solid-phase extraction combined with high performance liquid chromatography was used for the determination of nine sulphonamides in milk samples. The extraction and cleanup via silica-based magnetic adsorbent dispersion in milk samples followed by the magnetic isolation and desorption of the analytes using NaOH-methanol. Three different magnetic phenyl silica adsorbents were synthesized by varying the molar ratio of phenyltrimethylsilane and tetramethylorthosilicate; these adsorbents were evaluated for sulphonamides retention in terms of their pH and degree of hydrophobicity. The optimal conditions were a pH of 6.0 and a magnetic:sorbent ratio of 2:1. Under optimal conditions, limits of detection ranging from 7 to 14 μg L(-1) were obtained. The method was validated according with the European Commision Decision 2002/657/EC. The proposed method was applied to analyse sulphonamides in 27 milk samples of different brands. Thirteen samples tested were positive for the presence of sulphonamides., (Copyright © 2014 Elsevier Ltd. All rights reserved.)
- Published
- 2014
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