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

作　　者：王同珍 阚广磊 郑宇丽 柯丽群 张婷 曹维强 WANG Tong-Zhen;KAN Guang-Lei;ZHENG Yu-Li;KE Li-Qun;ZHANG Ting;CAO Wei-Qiang(Consumer Testing Technology Co., Ltd, Dongguan 523000, China;Shenzhen Consumer Testing Technology Co., Ltd, Shenzhen 518000, China)

机构地区：[1]东莞市中鼎检测技术有限公司,东莞523000 [2]深圳市中鼎检测技术有限公司,深圳51800

出　　处：《食品安全质量检测学报》2018年第13期3267-3274,共8页Journal of Food Safety and Quality

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1.997μg/kg、2.023μg/kg时,测定结果的扩展不确定分别为0.241μg/kg、0.256μg/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。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 introductio n 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.

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 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]