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The uncertainty of UV-Vis spectrophotometric and FAAS analysis for the determination of iron in pharmaceutical products

机译:紫外-可见分光光度法和FAAS分析法测定药品中铁的不确定度

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摘要

UV-Vis spectrophotometric (UV-Vis) and flame atomic absorption spectrometric (FAAS) analysis for iron determination in a pharmaceutical product were compared in terms of uncertainty budgets. Both methods are selective for iron; no interference due to other components present in the matrix was found. The results for the UV-Vis and FAAS methods were 11.4 +/- 0.5 mg and 11.9 +/- 0.8 mg, respectively, of iron per tablet (at a 95% confidence level). In both methods, the main uncertainty contribution is that due to the calibration function's non-linearity (0.32 mg and 0.46 mg or 42% and 31% of the standard uncertainty in the case of UV-Vis and FAAS, respectively). This finding encourages us to take uncertainty due to non-linearity into account in uncertainty estimations, even for highly linear methods like UV-Vis. In the ranking of uncertainty contributors, non-linearity is followed by instrument drift in the FAAS method and the uncertainty of volumetric measurements in UV-Vis. In particular, pipetting contributes about 16% of the uncertainty for UV-Vis spectrometry and 10% for FAAS, which is somewhat larger than that usually assumed. The uncertainty contributions of the two methods are compared and discussed in terms of experimental conditions.
机译:根据不确定性预算,比较了用于药品中铁测定的紫外可见分光光度法(UV-Vis)和火焰原子吸收分光光度法(FAAS)分析。两种方法都对铁具有选择性。没有发现由于基质中存在的其他成分引起的干扰。 UV-Vis和FAAS方法的结果是每片铁的铁含量分别为11.4 +/- 0.5 mg和11.9 +/- 0.8 mg(置信水平为95%)。在这两种方法中,主要的不确定性贡献是由于校准函数的非线性(对于UV-Vis和FAAS,分别为0.32 mg和0.46 mg或标准不确定性的42%和31%)。这一发现鼓励我们在不确定性估计中考虑非线性因素带来的不确定性,即使对于像UV-Vis这样的高度线性方法也是如此。在不确定性因素的排名中,非线性因素是FAAS方法中的仪器漂移以及UV-Vis中体积测量的不确定性。尤其是,移液对UV-Vis光谱的不确定度约占16%,对于FAAS的不确定度约占10%,这比通常假定的要大一些。根据实验条件对两种方法的不确定性贡献进行了比较和讨论。

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