Artigo sulfonamidas

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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 2012Received 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. Thebest 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 mgkgÀ1), 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)were supplied by SigmaeAldrich (St Louis, MO, USA). Finally, sulfamethoxazole (99.0%) was furnished by Globe Química (Cosmópolis, SP, Brazil). Individual stock solutions were prepared at 1.00 g LÀ1 in methanol and stored at À20 Æ 2  C in a freezer. The working solutions were prepared as appropriate dilutions of the stock solutions with Milli-Q water. 2.2. Instrumentation 2.2.1. Chromatographicconditions The HPLCeMS/MS system consisted of an Alliance 2795 (Micromass, Manchester, UK) chromatographer and a Quattro Premier XE (Micromass, Manchester, UK) triple quadrupole mass spectrometer. The separation of the sulfonamides was accomplished at 30  C with a Zorbax Eclipse XDB C-18 (dimensions: 4.6 Â 150 mm, particle size: 5 mm) column (Agilent, Santa Clara, CA, USA). The flow rate andinjection volume were 0.3 mL minÀ1 and 50 mL, respectively. The mobile phases used were (A) formic acid 0.1% in water/acetonitrile (95:5 v/v) and (B) formic acid 0.1% in water/acetonitrile (5:95 v/v). The gradient elution program was as follows: A (90%)eB (10%) (5 min), A (80%)eB (20%) (4 min), A (50%)eB (50%) (3 min), A (20%)eB (80%) (3 min), and A (10%)eB (90%) (3 min). The total chromatography runtime was 18 min. 2.2.2. Mass spectrometric conditions Electrospray ionization was performed in the positive ion mode for all the analytes. The mass spectrometer was operated under the following conditions: capillary voltage 2.8 kV, source temperature 120  C, desolvation temperature 300  C, cone gas flow 46 L hÀ1, and desolvation gas flow 697 L hÀ1. In order to determine the m/z transitions, solutionsof each analyte at 10 mg LÀ1 in methanol:water (1:1 v/v) containing 0.01% (v/v) of formic acid were directly infused with a micro syringe (Hamilton, Reno, NV) at a flow rate of 10 mL minÀ1 into the mass spectrometer ion source. A summary of the precursor and product ions, collision energy, and dwell time achieved for each analyte is presented in Table 1.

2.3. Sample preparation Finely ground...