Trace analysis of sulfamethazine in animal feed, human urine, and wastewater by electron capture gas chromatography.

Sulfamethazine, a widely used antibacterial drug additive in feeds for swine, chickens, and cattle, was scheduled for toxicological evaluation because of potential human health hazards associated with its residues in edible animal tissues. Analytical chemical procedures that would ensure proper concentration, homogeneity, and stability of the drug in dosed feed and its safe usage during the animal studies were prerequisites for such toxicological tests. Electron capture gas chromatographic (EC/GC) methods were therefore devised for the analysis of sulfamethazine residues in animal feed, human urine, and wastewater at levels as low as 100, 10, and 10 ppb, respectively. Sample extracts were cleaned up by using liquid/liquid partitioning, and the extracts were subjected to two derivatizations followed by cleanup on a silica gel column. The derivatizations of sulfamethazine consisted of methylation followed by trifluoroacetylation of the primary amine function. Ancillary data concerning stability of the compound in animal feed, water, and as a dry residue on glass, extraction efficiencies, partition values with various solvents, and the analysis of residues in feed by high pressure liquid chromatography (HPLC) at levels as low as 1.0 ppm are presented.