Validating heteronuclear 2D quantitative NMR
Validating heteronuclear 2D quantitative NMR
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DOI：
10.1039/c6ay00111d
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发表时间：
2016-01-01
影响因子：
3.1
通讯作者：
Le Gresley, Adam
中科院分区：
文献类型：
--
作者：
Fardus-Reid, Fahmina;Warren, John;Le Gresley, Adam
核磁共振被广泛用于简单分析物的准确定量，如果仔细应用，可以产生SI可追溯的测量结果。由于光谱的复杂性和信号重叠，它在更复杂的分析物中的应用受到限制。由于其较高的分辨率，二维定量核磁共振开始成为一种可行的定量技术，用于这类复杂的分析物，但也带来了简单的一维定量核磁共振方法所不存在的各种实验偏差来源。为了声称二维核磁共振技术的SI可追溯性，这些偏差和额外的测量不确定度来源需要量化。这项工作评估了HSQC方法的应用，以最小的偏差执行定量分析，并以内部标准化的葡萄糖分析为例，评估实验和理论偏差之间的差异，并讨论以最小的方法验证确定测量不确定度的方法。
NMR is used extensively for accurate quantitation of simple analytes and can, with careful application, generate SI traceable measurements. Its application for more complex analytes is limited due to spectrum complexity and signal overlap. Due to its higher resolving power, 2D qNMR is starting to emerge as a viable quantitative technique for such complex analytes but brings with it a variety of sources of experimental bias not present in the simple 1D qNMR method. In order to claim SI traceability of 2D NMR techniques, these biases and additional sources of measurement uncertainty need to be quantified. This work evaluates the application of HSQC methods to perform quantitative analysis with minimal bias and using an internally standardised glucose assay as an example, to assess the variation between experimental and theoretical biases and discuss approaches to determine the measurement uncertainty with a minimum of method validation.