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Uncertainty Evaluation of Different Quantitative Calibration Methods for the Determination of Vitamin B12 in Infant Formula
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摘要: 本文以婴儿配方奶粉中的维生素B12测量为例，开展了标准加入法、标准加入同位素稀释质谱法、单点同位素稀释质谱法和校准曲线同位素稀释质谱法四种定量方法的不确定度评估。基于ISO-GUM指南等不确定度评估方法对四种定量方法进行不确定度量化评估，发现方法重复性和曲线拟合引入的不确定度为主要不确定度来源，且标准加入法评估得到的不确定度明显大于同位素内标法评估得到的不确定度。通过不同定量方法的比较研究，可以更有效地选择定量方式，提高测量精度。Abstract: In this study, take measurement of the vitamin B12 in infant formula as an example, measurement uncertainty was evaluated through four calibration methods, including standard addition method, standard addition-isotope dilution mass spectrometry method, single point isotope dilution mass spectrometry method, and standard calibration curve isotope dilution mass spectrometry method. The uncertainty evaluation of the four quantitative methods was assessed based on the ISO-GUM guidelines and other uncertainty assessment methods. The uncertainties introduced by the method of repeatability and curve fitting were the primary sources of uncertainty. Furthermore, the uncertainties obtained by the standard addition method were significantly more significant than those obtained by the isotope internal standard method. The comparative study of different quantification methods can lead to a more effective selection of quantification methods and improved measurement accuracy.
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图 1 不同定量方法不确定度及分量的比例
Figure 1. Uncertainty values of different quantitative methods with contribution from associate components
表 1 不同定量方法相关分量相对标准不确定度
Table 1. Relative standard uncertainty values of each components of the quantitative methods
不确定度来源 SA SA-IDMS SP-IDMS SCC-IDMS A类不确定度 重复性uref,rep 3.3% 1.1% 1.6% 1.3% B类不确定度 标准物质纯度uref,p 0.4% 0.4% 0.4% 0.4% 溶液制备与称量uref,w 0.1% 0.1% 0.1% 0.2% 校准曲线urel,cal 6.3% 2.5% / 2.6% 合成不确定度 7.2% 2.8% 1.7% 3.0% 扩展不确定度U(k=2) 14.4% 5.6% 3.4% 6.0% 
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