Artigo sulfonamidas

Food Control 28 (2012) 192e198

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Development and validation of a method for the determination of sulfonamides in animal feed by modified QuEChERS and LCeMS/MS analysis
Renata Pereira Lopes a, *, Érica Eustáquia de Freitas Passos b, Juarez Fabiano de Alkimim Filho b, Eugênia Azevedo Vargas b, Daniella Vasconcellos Augusti b, Rodinei Augusti b, ** a b

Departamento de Química, Universidade Federal de Minas Gerais, 31270-901, Belo Horizonte, MG, Brazil Laboratório Nacional Agropecuário (LANAGRO-MG), Ministério da Agricultura, Pecuária e Abastecimento (MAPA), Pedro Leopoldo, MG, Brazil

a r t i c l e i n f o
Article history: Received 17 February 2012 Received in revised form 6 April 2012 Accepted 25 April 2012 Keywords: Animal feed Sulfonamides QuEChERS HPLCeMS/MS

a b s t r a c t
A multiresidue method for the quantification of 13 sulfonamides in animal feed is described. It involves the application of a modified QuEChERS procedure followed by HPLCeMS/MS (high performance liquid chromatography coupled to tandem mass spectrometry) analysis. The best conditions for the extraction solution and PSA (primary secondary amine) mass were determined. After optimization, the method was validated according to the European Commission Decision 2002/657/EC. The validation levels employed were 25, 50 and 75 mg kgÀ1. Acceptable values were obtained for the following parameters: linearity (0.9864 < r2 < 0.9993), decision limit (50.4 mg kgÀ1 < CCa < 55.8 mg kgÀ1), detection capability (50.7 mg kgÀ199.0%). The following standards were purchased from Riedel de Haën (Seelze, Germany): sulfadimethoxine, sulfamethoxypyridazine, and sulfadoxine. On the other hand, sulfachloropyridazine, sulfamethazine, sulfaguanidine, sulfamerazine, sulfanilamide, sulfaquinoxaline, sulfisoxazole, sulfadiazine, sulfathiazole and sulfapyridine (used as an internal standard)