HPLC-柱后衍生荧光法测定水产品中河豚毒素含量结果的不确定度评定

Evaluation of Uncertainty in the Determination of Tetrodotoxin Content in Aquatic Products by HPLC-postcolumn Derivative Fluorescence Method

通过建立HPLC-柱后衍生荧光法测定水产品中河豚毒素含量的不确定度评定方法,量化分析测定结果的不确定度分量,并对各分量相对贡献进行比较。结果表明:测定结果的不确定度主要来源于标准品的校准过程、样品称量、实验过程移取及定容、样品重复实验误差、前处理过程中的回收率不同等。其中校准不确定度中标准溶液配制的不确定度贡献最多,称样量不确定度最小;当水产品中河豚毒素的含量为90.6μg/kg时,其扩展不确定度为0.69μg/kg(包含因子k=2)。

By establishing an uncertainty evaluation method for the determination of tetrodotoxin content in aquatic products using HPLC post column derivatization fluorescence method,the uncertainty components of the measurement results are quantitatively analyzed,and the relative contributions of each component are compared.The results indicate that the uncertainty of the measurement results mainly comes from the calibration process of the standard,sample weighing,experimental process transfer and volume determination,repeated experimental errors of the sample,and different recovery rates in the pre-treatment process.Among the calibration uncertainties,the uncertainty contribution of standard solution preparation is the highest,while the uncertainty of sample weighing is the lowest;When the content of tetrodotoxin in aquatic products is 90.6μg/kg,its expanded uncertainty is 0.69μg/kg(including factor k=2).