The Ion trap detector (ITD), in combination with a capillary gas chromatograph and under chemical ionization conditions, offers sufficient sensitivity to determine carbadoxrelated residues as the methyl ester derivative of quinoxaline- 2-carboxylic acid at 3 μg/kg or higher in porcine liver. A tetradeuterated internal standard of QME effectively compensates for losses incurred during sample preparation. The method produced mean levels of 3.3 (±0.5), 5.5 (±0.8), and 10.1 (±0.9) μg/kg for liver fortified at 3, 5, and 10 μg/kg. When applied to analysis of samples containing incurred residues of 14C-carbadox at the low μg/kg level, results were comparable to those obtained by reverse isotope dilution analysis.
A simple liquid chromatographic (LC) method was developed to determine and identify incurred morantel-related residues in bovine milk by converting them to 3-(3-methyl-2-thienyl) acrylic acid (CP-20,107). Key techniques in this method involve short-term digestion of milk in HC1 to release residues convertible to CP-20,107, isolation and alkaline hydrolysis of these precursors to CP-20,107, and recovery of the product for LC analysis. Photochemical conversion of CP-20,107 to its cisisomer and separation by LC identifies the residue. A homolog (pyrantel), which is used as an internal standard, is hydrolyzed to 3-(2- thienyl) acrylic acid. These acrylic acid isomers are readily resolved by LC. The method was evaluated over the 1-4 ppb (ng/mL) range for accuracy and precision to assess its utility for withdrawal studies. Bovine milk supplemented with morantel at 1,2, and 4 ppb and assayed in replicate (n = 7-8) over 4 trials gave mean values and standard deviations of 1.0 ± 0.11,2.0 ± 0.24, and 4.0 ± 0.44 ppb, respectively. A milk specimen containing physiologically incurred residues of morantel assayed 2.1 ± 0.19 ppb in replicate (n = 5).
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