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A novel,simple and robust method for the analysis of sulfonamides in fish farming water samples using column switching liquid chromatography
Authors:Mariana Azevedo Rosa  Henrique Dipe De Faria
Affiliation:Laboratory of Toxicant and Drug Analyses, Federal University of Alfenas – UNIFAL-MG, Alfenas, Minas Gerais, Brazil
Abstract:
A novel method for the online extraction and preconcentration of four sulfonamides was developed using column switching liquid chromatography. Sulfadiazine, sulfathiazole, sulfamethoxypyridazine and sulfamethoxazole were analysed in water samples and preconcentrated in a C18 guard column. Suitable validation parameters were obtained, such as precision, accuracy and relative recovery, in accordance with the validation guidelines of the Food and Drug Administration. Low limits of detection (0.05–0.09 µg L?1) and quantification (0.30 µg L?1, for all of them) were obtained. The quadratic polynomial model was used to adjust the calibration data, and the coefficients of determination were higher than 0.999 for all the analytes. The method was shown to be robust to the assayed parameters according to Youden’s test. The proposed method was successfully used to determine sulfonamides in 11 different fish farming water samples, in which sulfadiazine (0.732 µg L?1), sulfamethoxazole (0.531 µg L?1), sulfathiazole (0.546–1.856 µg L?1) and sulfamethoxypyridazine (0.369–1.509 µg L?1) were found.
Keywords:Column switching  fish farming water  liquid chromatography  preconcentration  sulfonamide
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