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 Evaluating of Determination of Tilmicosin Residue in Swine Muscle by High Performance Liquid Chromatography Spectrometry

关键词:  高效液相色谱  猪肉  替米考星  残留  不确定度

Key words:  High Performance Liquid Chromatography Spectrometry, swine muscle, tilmicosin, residue, Uncertainty

摘要:

[摘要] 本研究依据“农业部1025号公告-10-2008”《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、仪器峰面积、样品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±5.92 μg/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。

Abstract:

Abstract: According to “Announcement No. 1025-10-28 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±5.92 μg/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.