同位素稀释-超高效液相色谱-串联质谱法测定牛奶中玉米赤霉醇含量的不确定度分析

Uncertainty evaluation for determination of zearalanol in milk by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  玉米赤霉醇  超高效液相色谱-串联质谱法  不确定度  同位素稀释

英文关键词:zearalanol  ultra performance liquid chromatography-tandem mass spectrometry  uncertainty  isotope dilution

中文摘要:

      目的 评定同位素稀释-超高效液相色谱-串联质谱法测定牛奶中玉米赤霉醇残留方法的不确定度。方法 以牛奶为例, 对同位素稀释-超高效液相色谱-串联质谱法测定牛奶中玉米赤霉醇残留的不确定度进行评定, 包含标准溶液配制引入的不确定度、测量重复性引入的不确定度、测量回收率引入的不确定度、样品称量引入等的不确定度几方面。结果 牛奶中α-玉米赤霉醇、β-玉米赤霉醇的含量为1.997 μg/kg、2.023 μg/kg时, 测定结果的扩展不确定分别为0.241 μg/kg、0.256 μg/kg, k=2。结论 测量结果的不确定主要来源为测量重复性、测量回收率以及曲线拟合, 在实际检测工作中, 可通过增加平行样、标准工作液的测定次数, 提高检测人员的工作质量, 提高检测质量。

英文摘要:

      Objective To investigate the uncertainty evaluation for the determination of zearalanol residues in milk by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry. Methods In the case of milk, the uncertainty of the determination of zearalanol residues was evaluated by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry. The uncertainty of the standard solution preparation, uncertainty introduced in the measurement repeatability, uncertainty of the introduction of measurement recovery, and uncertainty introduced in sample weighing were included. Results When the content of α-zearalanol and β- zearalanol in milk were 1.997 μg/kg and 2.023 μg/kg, respectively, the extended uncertainty were 0.241 μg/kg and 0.256 μg/kg with k=2, respectively. Conclusion The uncertainty of measurement results is mainly derived from measurement repeatability, measurement recovery and curve fitting. Therefore, in the actual testing work, the detection quality can be improved by increasing the number of parallel samples, determination time of standard working solution, so as to improve the quality of testers and reduce the uncertainty of measurement results.