Development and validation of an HPLC method for the determination of ten sulfonamide residues in milk according to 2002/657/EC.

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Tolika EP, Samanidou VF, Papadoyannis IN

Development and validation of an HPLC method for the determination of ten sulfonamide residues in milk according to 2002/657/EC.

J Sep Sci. 2011 Jul;34(14):1627-35. doi: 10.1002/jssc.201100171. Epub 2011 Jun 3.

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21644254 [ View in PubMed
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Abstract

A HPLC method with diode-array detection, at 265 nm, was developed and validated for the determination of ten sulfonamides (SAs): sulfadiazine (SDZ), sulfathiazine (STZ), sulfamethoxine (SMTH), sulfamethizole (SMZ), sulfamethoxypyridazine (SMPZ), sulfamonomethoxine (SMMX), sulfamethoxazole (SMXZ), sulfisoxazole (SIX), sulfadimethoxine (SDMX), and sulfaquinoxaline (SQX) in milk. A mixture of ethyl acetate, n-hexane, and isopropanol was used for the extraction of target analytes from milk. The mobile phase, a mixture of 0.1% v/v formic acid, CH(3) CN, and CH(3) OH was delivered to the analytical column under a gradient program. The procedure was validated according to the European Union regulation 2002/657/EC in terms of selectivity, stability, decision limit, detection capability, accuracy, and precision. Mean recoveries of sulfonamides from milk samples spiked at three concentration levels (0.5xMRL, 1xMRL, and 1.5xMRL) (MRL, maximum residue level) were 93.9-115.9% for SDZ, 97.8-102.9% for STZ, 94.6-107.0% for SMTH, 98.3-111.5% for SMZ, 95.3-108.4% for SMPZ, 97.9-106.0% for SMMX, 97.6-111.3% for SMXZ, 94.3-104.6% for SIX, 96.4-109.1% for SDMX, and 98.2-111.2% for SQX. All RSD values were lower than 8.8%. The decision limits CCa calculated by spiking 20 blank milk samples at MRL (100 mug/kg) ranged from 101.61 to 106.84 mug/kg, whereas the detection capability CCb ranged from 105.64 to 119.01 mug/kg.

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