title: Rapid sample preparation methods for analysis of residues of sulfamethazine and its N4-acetyl and desamino metabolites in swine tissue by HPLC.
abstract: Rapid sample preparation methods for the determination of sulfamethazine (SMZ) and its N4-acetyl and desamino metabolites in swine tissues at the 0.1 mg kg-1 level are presented. The methods use sonication-aided extraction with dichloromethane. For SMZ and N4-acetyl SMZ analysis extracts are cleaned up and concentrated on a silica disposable column followed by HPLC on a CP Spher C8 column using acetonitrile-sodium acetate buffer as the mobile phase. For desamino-SMZ analysis the extract was cleaned up and concentrated on a Florisil disposable column, followed by HPLC on a Nucleosil 5-CN column after formation of an ion-pair complex with 1-heptanesulfonic acid. For desamino SMZ peak identification by diode-array UV/VIS detection is also described. Mean recoveries from spiked tissue samples were about 87% (muscle) and 76% (kidney) for SMZ and N4-acetyl SMZ and about 70% for desamino SMZ.
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid; D007668:Kidney / Q000032:analysis; D009132:Muscles / Q000032:analysis; D013418:Sulfamethazine / Q000031:analogs & derivatives* / Q000032:analysis* / Q000378:metabolism; D013552:Swine; D000096926:Benzenesulfonamides
chemical_list: D013418:Sulfamethazine; C032633:N-acetylsulfamethazine; C028503:desaminosulfamethazine; D000096926:Benzenesulfonamides