通过液相色谱-串联质谱法（LC/MS/MS）测定从站立动物身上手术获取的牛血浆、尿液、口腔液体以及肾脏和肝脏活检样本中的磺胺二甲氧嘧啶和4-N-乙酰磺胺二甲氧嘧啶。
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.
作者信息
Li Hui, Smith Michelle L, Chiesa O Alberto, Kijak Philip J
机构信息
Food and Drug Administration, Center for Veterinary Medicine, Laurel, MD 20708, USA.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Jan 15;877(3):237-46. doi: 10.1016/j.jchromb.2008.12.015. Epub 2008 Dec 11.
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.
开发并验证了一种定量方法，用于测定牛组织和体液中磺胺二甲氧嘧啶（SDM）及其主要代谢物N-乙酰磺胺二甲氧嘧啶（AcSDM）的浓度。液相色谱/串联质谱法（LC/MS/MS）以SDM-d(4)作为内标（I.S.），给出了牛血浆、尿液、口腔液、肾脏和肝脏提取物中这两种分析物的定量结果。这些基质中两种分析物的定量下限（LLOQ）分别在血浆、尿液和口腔液中验证为2、100和5 ng/mL，在肾脏（皮质）和肝脏中均为10 ng/g。血浆的总体准确度（4个水平的平均值），SDM为104%，AcSDM为95%，标准偏差分别为9%（SDM）和15%（AcSDM）；尿液中，SDM为100%，AcSDM为106%，标准偏差分别为5%（SDM）和6%（AcSDM）；口腔液中，SDM为103%，AcSDM为103%，标准偏差分别为4%（SDM）和4%（AcSDM）；肾脏中，SDM为101%，AcSDM为111%，标准偏差分别为7%（SDM）和6%（AcSDM）；肝脏中，SDM为99%，AcSDM为115%，标准偏差分别为11%（SDM）和9%（AcSDM）。除尿液在通过LC/MS/MS分析前直接用缓冲液稀释外，使用C18固相萃取柱对这些基质进行净化。
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