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TITLE:  Determination of sulfadimethoxine and 4N-acetylsulfadimethoxine in bovine plasma, urine, oral fluid, and kidney and liver biopsy samples obtained surgically from standing animals by LC/MS/MS
AUTHORS:  Li H;Smith ML;Chiesa OA;Kijak PJ;
YEAR:  2009
JOURNAL ABBREV:  J Chromatogr B Analyt Technol Biomed Life Sci
JOURNAL FULL:  Journal of chromatography B, Analytical technologies in the biomedical and life sciences
VOLUME:  877
END PAGE:  246
KEYWORDS:  analogs & derivatives;analysis;Animals;Biopsy;blood;Cattle;chemistry;Chromatography,Liquid;Drug Stability;Food;Kidney;Linear Models;Liver;Mass Spectrometry;Reproducibility of Results;Saliva;Sensitivity and Specificity;Solid Phase Extraction;Sulfadimethoxine;Tandem Mass Spectrometry;urine;veterinary;Veterinary Medicine;
ABSTRACT:  A quantitative method was developed and validated to measure the concentration of sulfadimethoxine (SDM) and its major metabolite, (4)N-acetylsulfadimethoxine (AcSDM), in bovine tissues and body fluids. Liquid chromatography/tandem mass spectrometry (LC/MS/MS) gave quantitative results for these two analytes in extracts from bovine plasma, urine, oral fluid, kidney, and liver, using SDM-d(4) as internal standard (I.S.). The lower limit of quantitation (LLOQ) for both analytes in these matrices was validated at 2, 100, and 5 ng/mL in plasma, urine, and oral fluid respectively, and 10 ng/g in both kidney (cortex) and liver. The overall accuracy (average of 4 levels) is, for plasma, 104% (SDM) and 95% (AcSDM), with standard deviation of 9% (SDM) and 15% (AcSDM); for urine, 100% (SDM) and 106% (AcSDM), with standard deviation of 5% (SDM) and 6% (AcSDM); for oral fluid, 103% (SDM) and 103% (AcSDM), with standard deviation of 4% (SDM) and 4% (AcSDM); for kidney, 101% (SDM) and 111% (AcSDM), with standard deviation of 7% (SDM) and 6% (AcSDM); and for liver, 99% (SDM) and 115% (AcSDM), with standard deviation of 11% (SDM) and 9% (AcSDM). C18 SPE cartridges were used to clean-up these matrices, except for urine which was diluted directly with buffer before analysis by LC/MS/MS
AFFILIATIONS:  Food and Drug Administration, Center for Veterinary Medicine, Laurel, MD 20708, USA. hui.li@fda.hhs.gov