同位素稀释液相色谱-串联质谱法测定小麦中脱氧雪腐镰刀菌烯醇含量的不确定度评价

Uncertainty Evaluation of Deoxynivalenol Content in Wheat Determined by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

采用同位素稀释液相色谱-串联质谱法测定小麦中脱氧雪腐镰刀菌烯醇,对测定过程中可能引入的不确定度进行分析评定,为建立有效的质量控制方法提供参考。结果表明:小麦中脱氧雪腐镰刀菌烯醇含量为306μg/kg时,其扩展不确定度为59μg/kg(k=2),影响检测结果不确定度的因素主要是标准溶液配制,其次是样品称量和样品基质,而样品提取及定容、标准曲线拟合及测量重复性等引入的不确定度较小。

The possible uncertainties in the determination of deoxynivalenol in wheat by isotope dilution liquid chromatography-tandem mass spectrometry were analyzed and evaluated to provide reference for the establishment of effective quality control methods.The results indicated that when the content of deoxynivalenol in wheat was 306μg/kg,the expanded uncertainty was 59μg/kg(k=2),the main factor affecting the uncertainty was the preparation of standard solution,followed by sample weighing and sample matrix,while the uncertainty introduced by sample extraction and constant volume,standard curve fitting and measurement repeatability was small.