水蒸気蒸留およびHPLCによる食品中のソルビン酸分析の不確かさおよび頑健性
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Japanese official method for sorbic acid determination in food samples was evaluated for its measurement uncertainty and robustness. Smoke-dried cuttlefish was used as a model food sample. As trueness estimated in terms of recovery with spiked blank sample was within the acceptable range, within-laboratory reproducibility based on repeated independent analyses of the sample with incurred analyte at about half of the regulatory standard was thought to be the good estimate of measurement uncertainty. Robustness of steam distillation procedure with respect to seven factors such as weight of the sample, speed of distillation, final volume of distillate was evaluated according to Plackett-Burman experimental design, while reproducibility of HPLC procedure was by analysing the data of repeated independent determinations of the extract by two-way nested ANOVA considering isolation columns and calibration curves as two factors. The distillation procedure was found to be quite robust against the chosen modifications of various factors, and most part of the HPLC procedure variability was attributable to the variation of calibration curves. As the method is used for analysis of a range of sample matrices and analyte concentrations, data of sorbic acid determinations of spiked samples that consisted of various matrices and various concentrations were evaluated as a whole. The recovery rates were within the range of 70% to 100%, and relative standard deviations of repeatability were all within the acceptable ranges calculated from Horwitz equation. It seemed that variability of mean recovery rates would be a useful parameter to evaluate equivalence between different methods.
- 2012-12-21
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- 水蒸気蒸留およびHPLCによる食品中のソルビン酸分析の不確かさおよび頑健性
- 水蒸気蒸留およびHPLCによる食品中のソルビン酸分析の不確かさおよび頑健性
- 水蒸気蒸留およびHPLCによる食品中のソルビン酸分析の不確かさおよび頑健性