论文部分内容阅读
目的通过超高效液相色谱-串联质谱法(UPLC-MS/MS)测定动物源性食品中氯霉素的残留量,给出不确定度,建立动物源性食品中氯霉素残留量的不确定度评定方法。方法试样中氯霉素经水溶解,用乙酸乙酯提取后用UPLC-MS/MS测定,采用内标法定量。分析动物源性食品中氯霉素残留量的测定程序,绘制不确定度因果图,识别和分析不确定度来源,量化不确定度,计算合成不确定度。结果动物源性食品中氯霉素残留量为(6.036±0.616)μg/kg,k=2。本实验中不确定度的来源主要是标准溶液浓度、标准曲线拟合、待测样品的制备时、回收率和样品测定的重复性等。结论本实验中最大的不确定度来源于标准曲线的配制,容易偏高的回收率,不确定度分量因采用内标校正得到有效控制。
OBJECTIVE To determine the residual amount of chloramphenicol in animal food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), and to give the uncertainty, and to establish the limit of chloramphenicol residues in animal-derived food Determination of the degree of certainty. Methods Chloramphenicol was dissolved in water and extracted with ethyl acetate, then determined by UPLC-MS / MS and quantified by internal standard method. The procedure for the determination of chloramphenicol residues in animal-derived foods was analyzed, the causality map of uncertainty was drawn, the sources of uncertainty were identified and analyzed, the uncertainty of quantification was calculated, and the synthesis uncertainty was calculated. Results The residues of chloramphenicol in animal-derived food were (6.036 ± 0.616) μg / kg and k = 2. The main sources of uncertainty in this experiment are standard solution concentration, standard curve fitting, sample preparation, recovery, and repeatability of sample determination. Conclusion The maximum uncertainty in this experiment comes from the formulation of the standard curve, which is prone to high recovery rate. The uncertainty component is effectively controlled by internal standard calibration.