高效液相色谱法检测猪肉中替米考星残留量不确定度评定

Uncertainty Evaluation for the Determination of Tilmicosin Residue in Swine Muscle by High Performance Liquid Chromatography Spectrometry

本研究依据“农业部1025号公告-10^(-2)008”《动物性食品中替米考星残留检测高效液相色谱法》,对猪肉中替米考星的残留量进行了测量不确定度评定。共涉及对照溶液配制、样品称量、样品溶液制备以及仪器峰面积、样品回收率5个评定分量,结果显示:检测替米考星的相对标准不确定度分量依次为3.09×10^(-2)、5.78×10^(-3)、4.00×10^(-3)、2.31×10^(-2)和1.34×10^(-2),其中对照溶液配制、仪器峰面积、回收率不确定度分量对合成不确定度的贡献较高。兽药替米考星在猪肉样品中的检测结果在95%的置信限(k=2)内可表示为:71.6±5.92μg/kg(k=2)。不确定度评定结果为系统评价高效液相色谱法检测猪肉中替米考星残留结果的准确程度和方法的可靠性提供依据。

According to“Announcement No.1025-10^(-2)008 of the Ministry of Agriculture of determination of tilmicosin residue in swine muscle by high performance liquid chromatography spectrometry”,the uncertainties of tilmicosin residues in swine muscle were evaluated.Five evaluation components,including standard solution,sample weighing,sample solution,sample solution peak area and recovery were studied.Results showed that the relative combined standard uncertainties of determination of tilmicosin were 3.09×10^(-2),5.78×10^(-3),4.00×10^(-3),2.31×10^(-2)and 1.34×10^(-2),respectively.Three evaluation components of standard solution,sample solution peak area and recovery had greater contribution in the combined uncertainty of tilmicosin residue.In this study,the detection results of tilmicosin in swine muscle samples in 95%confidence interval could be expressed as tilmicosin 71.6±5.92μg/kg(k=2).The uncertainty assessment result provided the technical supplement for the accuracy and reliability of the determination of tilmicosin residue in swine muscle by high performance liquid chromatography spectrometry.