摘要
对高效液相色谱-串联质谱法测定鱼肉中4种有机磷农药残留量进行不确定度评定.按照《GB 31656.8-2021食品安全国家标准水产品中有机磷类药物残留量的测定液相色谱-串联质谱法》测定鱼肉中倍硫磷、马拉硫磷、敌敌畏、蝇毒磷4种有机磷农药残留量,利用方法确认的数据评定测量不确定度.建立数学模型,分析样品称量、标准品纯度、计量器具、标准曲线拟合、回收率、精密度、仪器设备等因素并量化.当样品中倍硫磷、马拉硫磷、敌敌畏、蝇毒磷的含量分别为46.43、94.96、40.91、94.34 µg/kg水平时,扩展不确定度分别为8.90、18.49、8.27、20.16 µg/kg.评定结果表明,本方法的不确定度来源主要是标准曲线拟合、计量器具、精密度和回收率,评定的结果可以为科学评价鱼肉中有机磷药物残留测量结果的准确性提供依据.
Abstract
The uncertainty of determination of four organophosphorus pesticide residues in fish by high performance liquid chromatography-tandem mass spectrometry was evaluated.According to GB 31656.8-2021 National Food Safety Standard-Determination of organophosphorus pesticide residues in aquatic product-Liquid Chromatography-Tandem Mass Spectrometry,the residues of fenthion,malathion,dichlorvos and coumaphos in fish were determined,and the measurement uncertainty was evaluated by the data confirmed by the method.Establish mathematical model,analyze and quantify factors such as sample weighing,purity of standard,measuring instruments,standard curve fitting,recovery rate,precision,instruments and equipment,etc.When the contents of fenthion,malathion,di-chlorvos and coumaphos in the sample were 46.43,94.96,40.91,94.34 µg/kg,the expanded uncertainties were 8.90,18.49,8.27,20.16 μg/kg,respectively.The evaluation results show that the uncertainty of this method mainly comes from standard curve fitting,measuring instruments,precision and recovery rate,and the evaluation results can provide a basis for scientific evaluation of the accuracy of the measurement results of organophosphorus drug residues in fish.
基金项目
吉林省科技创新平台和人才专项(20220505044ZP)
NETL
NSTL
万方数据