Development and Validation of an HPLC Method for the Simultaneous Determination of Ten Sulfonamide Residues in Bovine, Porcine and Chicken Tissues According to 2002/657/EC

Evanthia      P. Tolika; Victoria      F. Samanidou; Ioannis      N. Papadoyannis

Abstract

An HPLC method with a diode-array-detector set at 265 nm, which was developed and validated for the simultaneous determination of ten sulfonamides, in bovine, porcine and chicken tissue is presented. The separation was achieved on an analytical column, Kromasil, C18 5 μm, 250 x 4 mm at ambient temperature. The mobile phase, a mixture of 0.1% formic acid, CH3CN and CH3OH, was delivered by a gradient program. The examined sulfonamides, (sulfadiazine (SDZ), sulfathiazine (STZ), sulfamethoxine (SMTH), sulfamethizole (SMZ), sulfamethoxypyridazine (SMPZ), sulfamonomethoxine (SMMX), sulfamethoxazole (SMXZ), sulfisoxazole (SIX), sulfadimethoxine (SDMX) and sulfaquinoxaline (SQX)) were extracted from the tissues using mixtures of ethyl acetate, water and acetonitrile. SPE was necessary for further purification. The method was validated according to the Decision 2002/657/EC, determining selectivity, stability, decision limit, detection capability, accuracy, linearity and precision. Overall recoveries ranged from 90.1 to 115.1%. All RSD values were lower than 10.0%. The decision limits CCα ranged for bovine tissue from 103.68 to 112.36 μg/kg, for porcine tissue from 108.13 to 110.13 μg/kg and for chicken tissue from 103.93 to 111.92 μg/kg, while detection capability CCβ ranged from 111.62 to 121.26 μg/kg, from 111.74 to 124.83 μg/kg and from 111.32 to 119.86 μg/kg respectively.

Keywords: 2002/657/EC, Bovine, Chicken, HPLC, Porcine, Residues, SPE, Sulfonamides, Tissues, Validation