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目的评定超高液相色谱-串联质谱法测定猪肉中8种喹诺酮类兽药残留量的不确定度。方法根据JJF 1135-2005《化学分析测量不确定度评定》和JJF 1059.1-2012《测量不确定度评定与表示》中的有关规定,建立不确定度的数学模型,逐层对不确定度进行分析。结果添加量为1.0μg/kg时,8种喹诺酮类兽药残留量测定的相对标准不确定度为2.77%~6.65%;添加量为2.0μg/kg时,8种喹诺酮类兽药残留量测定的相对标准不确定度为1.69%~6.67%;添加量为4.0μg/kg时,8种喹诺酮类兽药残留量测定的相对标准不确定度为1.31%~5.43%。结论在实际检测中,提高天平精度及定容精度,控制标准溶液配制过程,提高检验员工作质量和效率均可降低引入的不确定度,使检测结果更可靠。
OBJECTIVE To assess the uncertainty of 8 quinolone residues in pork by ultra performance liquid chromatography-tandem mass spectrometry. Methods Based on the JJF 1135-2005 “Evaluation of Uncertainty in Chemical Analysis Measurement” and JJF 1059.1-2012 “Evaluation and Expression of Uncertainty in Measurement”, a mathematical model of uncertainty was established and the uncertainty was analyzed layer by layer . Results The relative standard uncertainty of the determination of 8 quinolone veterinary drugs was 2.77% -6.65% when the dosage was 1.0 μg / kg. The relative standard uncertainty of 8 quinolone veterinary drugs was 2.07 The standard uncertainty was 1.69% ~ 6.67%. The relative standard uncertainty of the determination of 8 quinolone veterinary drugs was 1.31% ~ 5.43% at the dosage of 4.0μg / kg. Conclusion In the actual test, the accuracy and volumetric accuracy of the balance are improved, the preparation process of the standard solution is controlled, the quality and efficiency of the inspector can be reduced to reduce the uncertainty introduced, and the test results are more reliable.