液相色谱-串联质谱法测定鲈鱼中磺胺二甲嘧啶的不确定度评定

Uncertainty evaluation of determination of sulfamethazine in perch by liquid chromatography-tandem mass spectrometry

采用液相色谱-串联质谱法对鲈鱼样品中磺胺二甲嘧啶进行检测,对其不确定度进行评定。以氘代磺胺邻二甲氧嘧啶为内标,样品经酸化乙腈提取后,用液相色谱-串联质谱法对鲈鱼样品中磺胺二甲嘧啶进行检测,建立数学模型,分析不确定度来源,对其测量不确定度进行评定。结果表明:鲈鱼样品中磺胺二甲嘧啶含量为166μg/kg;扩展不确定度为21μg/kg,k=2;结果可表示为(166±21)μg/kg,k=2。在测定鲈鱼样品中磺胺二甲嘧啶时,不确定度来源主要有重复测量引入、回收率引入、校正曲线拟合引入、校正溶液的配制过程引入、前处理操作引入以及检测仪器引入等。其中校正曲线拟合、校正溶液配制和检测仪器对不确定度的贡献最大。

Sulfamethazine in perch samples was detected by liquid chromatography-tandem mass spectrometry,and its uncertainty was evaluated.Deuterated sulfadiazine was used as the internal standard,and the samples were extracted by acidified acetonitrile,and the sulfamethazine in perch was detected by liquid chromatography-tandem mass spectrometry,anda mathematical model was established,and the sources of uncertainty was analyzed,and the measurement uncertainty was evaluated.The results showed that content of sulfamethazine in perch samples was 166μg/kg,and the expanded uncertainty was 21μg/kg,k=2,and the results could be expressed as(166±21)μg/kg,k=2.In the determination of sulfamethazine in perch samples,the main sources of uncertainty mainly included the introduction of repeated measurement,the introduction of recovery rate,the introduction of correction curve fitting,the introduction of preparation process of correction solution,the introduction of pretreatment operation,and the introduction of detection instrument.The correction curve fitting,correction solution preparation and detection instruments contributed the most to the uncertainty.