Abstract

A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet (Oreochromis niloticus) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity (r ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g−1 and 5 ng·g−1, respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CCα 102.6–120.0 ng·g−1 and 70 ng·g−1 for sulfonamides and trimethoprim, respectively) and detection capability (CCβ 111.7–140.1 ng·g−1 and 89.9 ng·g−1 for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies.

Highlights

  • Brazil is one of the five largest veterinary markets in the world, and aquaculture, in particular fish farming, is the fastest growing sector of animal food production in the country [1, 2]

  • Results and Discussion e representative sulfonamide veterinary drugs were chosen based on a study of their use in fish farming around the world, those monitored by the Brazilian National Plan for Control of Residues and Contaminants (PNCRC/Fish) of the Brazilian Ministry of Agriculture, Livestock, and Food Supply and those used for other animal species that could potentially be illegally employed in fish farming. us, sulfamethazine, sulfathiazole, sulfadimethoxine, sulfamerazine, sulfamethoxazole, sulfapyridine, sulfamethoxypyridazine, and trimethoprim were selected. e maximum residue limit (MRL) adopted for all the sulfonamides was 100 μg·kg−1, and 50 μg·kg−1 for trimethoprim [7]

  • Dispersive solid-phase extraction (d-SPE) technique and QuEChERS have been previously used for the determination of veterinary drug residues in animal fluids and tissues [16, 27, 28], but not for the concomitant determination of sulfonamides and trimethoprim in fish fillet

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Summary

Introduction

Brazil is one of the five largest veterinary markets in the world, and aquaculture, in particular fish farming, is the fastest growing sector of animal food production in the country [1, 2]. Antimicrobials, including sulfonamides, are used for the treatment of bacterial diseases. Sulfonamides (Figure 1) belong to an important group of synthetic antimicrobial agents that have been used in human and veterinary medicine for over 60 years. These drugs have been extensively employed in animals intended to produce food for human consumption since it is practically impossible to keep the production environment free of pathogenic organisms. Sulfonamide residues are a major concern because of their potential risk to human health by development of bacterial resistance and adverse effects, such as allergic reactions, in hypersensitive people [4]

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