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Determination of Sulfathiazole in Type C Medicated Swine Feed by Reversed-Phase Liquid Chromatography with Post-Column Derivatization

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A convenient method was developed for determination of sulfathiazole (STZ) in Type C medicated swine feed by reversed-phase liquid chromatography (LC) with post-column derivatization. Addition of extractant solution (0.2N HCl and 1.5% diethylamine in 25% methanol) and an internal standard (IS), sulfamethylthiazole (SMZ), to 5 g sample was followed by mechanical shaking for 1 h. The extract was clarified by chilling, centrifugation, and filtering before injection onto a C18 reversed-phase column. The mobile phase components were 2% acetic acid and 1:1 acetonitrile–methanol (83 + 17%, v/v). Run time was about 20 min. Determination and, largely, the method's selectivity were based on detection at 450 nm of the derivative formed by the post-column reaction of dimethylaminobenzaldehyde with the primary amine of the analyte and IS. The IS, SMZ, differs from STZ by a single substituent methyl group, is stable, and is readily resolved from STZ. Although SMZ is not commercially available, it can be synthesized with relative ease from purchased reagents and will be supplied by the authors to interested laboratories. In single-laboratory validation, linearity was demonstrated over the range of 0.055–550 μg/mL, well beyond the target concentration of 5.5 μg/mL. The estimated limit of detection was 0.04 μg/mL; the calculated limit of quantitation was 0.13 μg/mL (feed concentration of 2.4 g/T or 2.7 mg/kg). Wet-spiking trials with a variety of swine feed matrixes showed recovery to be 100–102% for the intended concentration range, 50–200 g/T, with coefficient of variation (CV) <2%. The method ruggedness was verified with an overall CV of 2.9%.
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Document Type: Research Article

Affiliations: Office of Indiana State Chemist, Purdue University, 175 S University St, West Lafayette, IN 47907

Publication date: 2003-07-01

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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