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.

Thermodynamic analysis of the thermal stability of sulphonamides in milk using liquid chromatography tandem mass spectrometry detection

“…Improper use of SAs, such as excessive administration and an inadequate withdrawal period, may result in sulphonamide residues in milk. These residues are of great public health interest given the risk of developing the growth of an antibiotic-resistant bacteria strain, thus rendering inefficient this type of drug for therapeutic use (Chung, Lee, Chung, & Lee, 2009;Haagsma, Pluijmakers, Aets, & Beek, 1989). Moreover, SA residues are of particular concern given the potential carcinogenic character of some substances, such as sulfamethazine (Littelefield, Sheldon, Allen, & Gaylor, 1990).…”

Validation of a liquid chromatography with ultraviolet detection methodology for the determination of sulfonamides in bovine milk according to 2002/657/EC

“…The presence of sulfonamide residues in milk intended for human consumption is of toxicological and regulatory concern. Some of the compounds such as sulfamethazine are carcinogen (Littlefield, Sheldon, Allen, & Gaylor, 1990), and all of them can promote occurrence of the antibioticresistant bacteria, which leads to inefficiency of this medicine for the therapeutic use (Haagsma, Pluijmakers, Aerts, & Beek, 1987), as well as severe allergic reactions.…”

Use of chemometric techniques to design a microbiological method for sulfonamide detection in milk

“…The presence of these antimicrobials can produce a risk for consumers' health (Haagsma et al 1989) and technological problems for the dairy industry (Berruga et al 2007).…”

“…Several authors (Nouws et al 1999;Althaus et al 2009) have proposed the use of a Microbiologic Multiplate System (MMPS) with Petri dishes to identify correctly the antimicrobial families in milk. Bacillus subtilis is used as the test strain for the detection of sulphonamides as being sensitive enough (Haagsma et al 1989). However, the analysis done in Petri dishes involve long incubation times to identify SAs (18-24 h) and require personnel trained to work in microbiology.…”