title: Development and validation of an HPLC method for the determination of ten sulfonamide residues in milk according to 2002/657/EC.
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 CCa 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 CCb ranged from 105.64 to 119.01 μg/kg.
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
authors.forename: Evanthia P
authors.initials: EP
authors.lastname: Tolika
authors.forename: Victoria F
authors.initials: VF
authors.lastname: Samanidou
authors.forename: Ioannis N
authors.initials: IN
authors.lastname: Papadoyannis
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005062:European Union; D005506:Food Contamination / Q000032:analysis; D008892:Milk / Q000737:chemistry*; D013449:Sulfonamides / Q000032:analysis*; D019155:Veterinary Drugs / Q000032:analysis
chemical_list: D000900:Anti-Bacterial Agents; D013449:Sulfonamides; D019155:Veterinary Drugs