Ali_1993_J.AOAC.Int_76_1309

To optimize conditions for sample collection, preparation, storage, and analysis and to assure the validity of our previously published liquid chromatographic (LC) method for carbamate analysis in tissue, stabilities of 16 N-methylcarbamates in beef, duck, and chicken liver tissues were studied by using 2 sampling protocols. Tissue samples were fortified at room temperature to a concentration 5 to 10 times greater than either the Environmental Protection Agency tolerance level for each compound (if established) or the concentration used in the previously published method. Thereafter, samples were continuously frozen at -4 degrees C for varying time intervals. In the first study, samples were analyzed one day (initial) and 0.5, 1, 1.5, 2, 3, 4, 5, and 6 months after fortification. In the second study, samples were analyzed one day (initial) and 0.5, 1, 2, 3, and 6 months after fortification. For each residue and species, a minimum of 4 samples were analyzed by LC at each point in time, and the mean represented analyte concentration at the end of each time interval. Rates of residue depletion varied among analytes and among species. Depletion rates were greater in duck livers than in beef livers. Methomyl and oxamyl were depleted completely within 2 weeks. Between 2 and 6 months after sample fortification, residue depletions to levels below detection limits were observed for aldicarb, aldicarb sulfoxide, aldicarb sulfone, dioxacarb, promecarb, propoxur, and bendiocarb. The initial loss of certain carbamates during sample preparation in tissues exposed to room temperature for up to 8 h was greater than the subsequent rate of loss. Results indicate that cryogenic conditions are required for sample preparation and storage.