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

✍ Scribed by Evanthia P. Tolika; Victoria F. Samanidou; Ioannis N. Papadoyannis

• Publisher: John Wiley and Sons
• Year: 2011
• Tongue: English
• Weight: 199 KB
• Volume: 34
• Category: Article
• ISSN: 1615-9306
• DOI: 10.1002/jssc.201100171

✦ Synopsis

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 (0.5×MRL, 1×MRL, and 1.5×MRL) (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 CC__a__ calculated by spiking 20 blank milk samples at MRL (100 μg/kg) ranged from 101.61 to 106.84 μg/kg, whereas the detection capability CC__b__ ranged from 105.64 to 119.01 μg/kg.