title: Development and validation of a confirmatory method for the determination of sulphonamides in milk by liquid chromatography with diode array detection.
abstract: A simple and rapid multiresidue method for the determination of seven sulphonamides residues (sulfadiazine, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine and sulfaquinoxaline) in milk samples was developed and validated. The drugs were extracted with a mixture chloroform/acetone and simply cleaned up on a cation exchange solid phase extraction column. The analytes determination was carried out using liquid chromatography with diode array detection (DAD). The procedure has validated as a quantitative confirmatory method according to the European Union (EU) Decision 2002/657/EC. The developed method shows good linearity, specificity, precision (repeatability and intra-laboratory reproducibility), ruggedness and is able to confirm each sulphonamide residue above 30mugkg(-1). Decision limits (CCalpha) around 110mugkg(-1) and recovery above 56% were obtained for all the analytes. The results of the validation process demonstrate that the method is suitable for application, as confirmatory method, in European Union statutory veterinary drug residue surveillance programmes. In addition, a hypothetical situation of sample judgement (compliance or not) in the case in which, at the same time, two different sulphonamides are found, is discussed.
authors.affiliation: Istituto Zooprofilattico Sperimentale della Lombardia e dell'Emilia Romagna, "B. Ubertini", Via Bianchi 9, 25124 Brescia, Italy.
authors.forename: Valentina
authors.initials: V
authors.lastname: Gamba
authors.forename: Chiara
authors.initials: C
authors.lastname: Terzano
authors.forename: Laura
authors.initials: L
authors.lastname: Fioroni
authors.forename: Simone
authors.initials: S
authors.lastname: Moretti
authors.forename: Guglielmo
authors.initials: G
authors.lastname: Dusi
authors.forename: Roberta
authors.initials: R
authors.lastname: Galarini
mesh_terms: D000096:Acetone / Q000737:chemistry; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D002725:Chloroform / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D004350:Drug Residues / Q000032:analysis* / Q000302:isolation & purification; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D013449:Sulfonamides / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D000900:Anti-Bacterial Agents; D013449:Sulfonamides; D000096:Acetone; D002725:Chloroform