A rapid LC-MS/MS method, using a triple quadrupole/ linear ion trap mass spectrometer, was developed for determination of penitrem A and roquefortine C in serum and urine samples. Penitrem A and roquefortine C were extracted from samples with methylene chloride. The extracts were injected onto a liquid chromatograph coupled with a hybrid triple quadrupole/ linear ion trap mass spectrometer. Seven replicate fortifications of serum at 0.001 mu g/g ( 1 ppb) each of penitrem A and roquefortine C gave average recoveries of 90% with 10% CV ( relative standard deviation) and 97% with 3% CV, respectively. Seven replicate fortifications of urine at 0.001 mu g/g ( 1 ppb) each of penitrem A and roquefortine C gave average recoveries of 98% with 12% CV and 100% with 6% CV, respectively. This is the first report of a positive mass spectrometric identification and quantitation of both compounds in urine and serum samples from dog intoxication cases.
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