中文摘要：本研究比较了人尿中10种镰刀菌毒素和代谢物的简单高效的样品制备方法，即分散液液微萃取和盐析液-液萃取，并评估了多个影响提取效率的参数。在最佳提取条件下，盐析液液萃取的准确度(84-96%)和精密度(<14%)高于分散液液微萃取。于是提出了基于盐析液-液萃取后接气相色谱-串联质谱的多生物标记方法。并在测定霉菌毒素偶联物前，用该方法初步研究了12个经β-葡糖苷酸酶处理前后的人尿样品。在83%的阳性样品中发现总脱氧雪腐镰刀菌烯醇（游离+偶联）的平均浓度为31.6μg/L。
外文摘要：Simple and highly efficient sample preparation procedures, namely, dispersive liquid-liquid microextraction and salting-out liquid-liquid extraction for the analysis of ten Fusarium mycotoxins and metabolites in human urine were compared. Various parameters affecting extraction efficiency were carefully evaluated. Under optimal extraction conditions, salting-out liquid-liquid extraction showed a better accuracy (84-96%) and precision (<14%) than dispersive liquid-liquid microextraction. Hence, a multi-biomarker method based on salting-out liquid-liquid extraction followed by gas chromatography with tandem mass spectrometry was proposed. Satisfactory results in terms of validation were achieved. The method resulted in low limits of detection and quantitation within the range of 0.12-4 and 0.25-8 μg/L, respectively. The method accuracy and precision were evaluated at three spiking levels (8, 25 and 100 μg/L) and the recoveries were in a range from 70 to 120% with relative standard deviations lower than 15%. Matrix effect was evaluated and matrix-matched calibrations were used for quantitation purpose. The developed method was applied in 12 human urine samples as a pilot study before and after sample treatment with β-glucuronidase before the analysis to quantify the mycotoxin conjugates. Total deoxynivalenol (free + conjugated) was found in 83% of samples at an average concentration in positive samples of 31.6 μg/L.
外文关键词：biomarkers；microextraction；mycotoxins；tandem mass spectrometry；urine
作者：Rodriguez-Carrasco, Y；Molto, JC；Manes, J；Berrada, H
作者单位：Univ Valencia
期刊名称：JOURNAL OF SEPARATION SCIENCE
期刊影响因子：2.741
出版年份：2017
出版刊次：7
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