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

Journal Article · Tue Dec 01 04:00:00 EST 1981 · J. Chromatogr. Sci.; (United States)

DOI:https://doi.org/10.1093/chromsci/19.12.625· OSTI ID:5594112

Holder, C L; Thompson, Jr, H C; Bowman, M C

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.

• Research Organization: DHHS, Food and Drug Administration, Jefferson, Arkansas
• OSTI ID: 5594112
• Journal Information: J. Chromatogr. Sci.; (United States), Journal Name: J. Chromatogr. Sci.; (United States) Vol. 19:12; ISSN JCHSB
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102* -- Chemical & Spectral Procedures
560306 -- Chemicals Metabolism & Toxicology-- Man-- (-1987)
63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTANT EFFECTS ON LIVING ORGS. AND BIOL. MAT.
AMINES
ANIMAL FEEDS
ANIMALS
ANTI-INFECTIVE AGENTS
ANTIBIOTICS
BIOLOGICAL MATERIALS
BIOLOGICAL WASTES
BODY FLUIDS
CHROMATOGRAPHY
DRUGS
ELECTRON-CAPTURE DETECTORS
FOOD
GAS CHROMATOGRAPHY
HAZARDS
HEALTH HAZARDS
HYDROGEN COMPOUNDS
LIQUID WASTES
MAMMALS
MAN
MATERIALS
MEASURING INSTRUMENTS
ORGANIC COMPOUNDS
ORGANIC SULFUR COMPOUNDS
OXYGEN COMPOUNDS
PRIMATES
RADIOMETRIC GAGES
SEPARATION PROCESSES
TRACE AMOUNTS
URINE
VERTEBRATES
WASTE WATER
WASTES
WATER