分散固相萃取-液相色谱法测定水果中氟吗啉残留量的不确定度

Uncertainty analysis of determination of flumorph in fruit by dispersive solid phase extraction and HPLC

对分散固相萃取法-液相色谱法测定水果中氟吗啉残留量过程进行分析,建立数学模型。评定各不确定度分量,合成标准不确定度,计算测定结果的扩展不确定度。结果表明:主要来源于标准系列溶液配制,样品的均匀性和样品前处理过程的一致性,以及标准曲线的拟合。当置信概率为95%,采用该方法测定试样中氟吗啉残留的扩展不确定度为0.18,则试样中茚虫威残留的检测结果可表示为(1.46±0.18)mg/kg(k=2)。

The uncertainty of measurement for flumorph residue in a sample by dispersive solid phase extraction and HPLC was evaluated. The mathematical model of measurement was set up. The different parts of uncertainty were analyzed, and the combined standard uncertainty and the expanded uncertainty of measurement results were calculated. The results showed that the main sources of uncertainties were the preparation of standard solutions, the fitted linear regression equation for the calibration curve, the uniformity of the samples and the consistency of sample pretreatment process. When the confidence probability was 95%, the expanded uncertainty in this analysis is 0.18 mg/kg with flumorph residue 1.46 mg/kg. So the flumorph residue in test sample can be expressed as （1.46＋0.18） mg/kg （k=2）.