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Evaluation of measurement uncertainty in EA–IRMS: for determination of δn 13C value and C-4 plant sugar content in adulterated honey

机译:EA–IRMS中测量不确定度的评估:用于测定掺假蜂蜜中的δn13C值和C-4植物糖含量

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摘要

In this study, the method for determining the stable carbon isotope ratio value was validated. Measurement uncertainty of stable carbon isotope ratio value of whole honey and its extracted protein derived from repeatability, reference gas, reference standards and calibration curve was calculated by applying the “bottom-up” approach according to Eurachem/CITAC guide. The expanded uncertainties for all results ranged from 0.14 to 0.19 ‰, with most of them between 0.15 and 0.16 ‰ (the coverage factor k = 2, the level of confidence p is approximately 95 %). The percentage contribution of each source to the relative combined uncertainty was calculated. The data indicated that calibration curves have more contribution to the relative combined uncertainty than repeatability and reference standards. On the other hand, the measurement uncertainty of C-4 sugar content in honey was estimated. Based on these results, 58 honey samples, such as acacia, chaste, Northeast China black bee, flowers and jujube honey, have been gathered to determine the C-4 plant sugar content adulteration in honey by elemental analyzer with an isotope ratio mass spectrometer. It can be found that all honey samples were not adulterated by C-4 plant sugar.
机译:本研究验证了确定稳定碳同位素比值的方法。根据Eurachem / CITAC指南,采用“自下而上”的方法,计算了整个蜂蜜及其提取蛋白质的可重复性,参考气体,参考标准品和校准曲线得出的稳定碳同位素比值的测量不确定度。所有结果的扩展不确定性范围为0.14至0.19‰,大多数不确定性在0.15至0.16‰之间(覆盖因子k = 2,置信度p约为95%)。计算每种来源对相对组合不确定性的百分比贡献。数据表明,与可重复性和参考标准品相比,校准曲线对相对组合不确定度的贡献更大。另一方面,估计了蜂蜜中C-4糖含量的测量不确定度。基于这些结果,已经收集了58种蜂蜜样品,如阿拉伯树胶,纯洁,东北黑蜂,花和枣蜂蜜,用元素分析仪和同位素比质谱仪测定了蜂蜜中C-4植物糖含量的掺假。可以发现,所有蜂蜜样品都没有被C-4植物糖掺假。

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