Determination of chlorinated methylthiobenzenes and their sulfoxides and sulfones in fish

Journal Article · · J. Assoc. Off. Anal. Chem.; (United States)

OSTI ID:5912055

Gardner, A M; Abramovitch, A

A procedure was developed to determine chlorinated methylthiobenzenes and their respective sulfur oxidation products in fish. Perch samples fortified at the 0.1 ppM level with 2,4,5-trichloromethylthiobenzene, pentachloromethylthiobenzene, and their sulfoxides and sulfones were extracted and cleaned up using an adaptation of the official AOAC method for multiple residues of organochlorine pesticides. The Florisil column cleanup was modified; 200 mL 6% petroleum ether-ethyl ether (PE-EE) eluted the methylthiobenzene, 200 mL 50% PE-EE eluted the sulfones, and 200 mL EE eluted the sulfoxides. Recoveries determined by electron capture (ECD) gas chromatography (GC) were 75-101% for the methylthiobenzenes and their sulfones and 63-93% for the sulfoxides. Co-extracted materials in the Florisil eluates that interfered with the ECD/GC quantitation were removed by partitioning the sulfoxides and sulfones into sulfuric acid and by this layer chromatography on silica gel, using methylene chloride-hexane (50 + 50) as the developing solvent. Seven fish samples containing residues of chlorinated benzenes or polychlorinated biphenyls (PCBs) were examined for chlorinated methylthiobenzenes, methylthio-PCBs, and their oxidation products by matching GC retention times obtained with the EC detector and a flame photometric detector operated in the sulfur mode. These analytes were not found in the fish samples above a detection level equivalent to 0.02 ppM 2,4,5-trichloromethylthiobenzene. 13 references, 1 figure, 3 tables.

• Research Organization: Food and Drug Administration, Washington, DC
• OSTI ID: 5912055
• Journal Information: J. Assoc. Off. Anal. Chem.; (United States), Journal Name: J. Assoc. Off. Anal. Chem.; (United States) Vol. 67:6; ISSN JANCA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102* -- Chemical & Spectral Procedures
ANIMALS
AQUATIC ORGANISMS
AROMATICS
CAPTURE
CHEMICAL ANALYSIS
CHLORINATED AROMATIC HYDROCARBONS
CHROMATOGRAPHY
DATA
ELECTRON CAPTURE
EXPERIMENTAL DATA
FISHES
GAS CHROMATOGRAPHY
HALOGENATED AROMATIC HYDROCARBONS
INFORMATION
NUMERICAL DATA
ORGANIC CHLORINE COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC HALOGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
SEPARATION PROCESSES
VERTEBRATES