Practical guide for accurate quantitative solution state NMR analysis

Practical guide for accurate quantitative solution state NMR analysis
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DOI:
10.1088/0026-1394/41/3/015
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发表时间:
2004-06-01
期刊:
影响因子:
2.4
通讯作者:
Maeda, T
Maeda, T
中科院分区:
工程技术3区
文献类型:
--
作者:
Saito, T;Nakaie, S;Maeda, T

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讨论并提出了定量溶液态核磁共振 (NMR) 分析中信号强度统计变化等实验条件的实用指南。统计分析表明,目标精度和实际脉冲间隔之间存在关系。需要设置音频滤波器的带宽,使所有感兴趣的信号落入滤波器中心部分的 80%。当满足这些条件时,可以通过确定单个光谱的信噪比(SN)来估计重复实验中信号区域的相对标准偏差(RSD)。当SN达到1000时,RSD随着SN的增加而变得恒定。在这样的条件下,定量 NMR 的准确度应优于 1%。
A practical guide to experimental conditions such as statistical variation of signal intensity on quantitative solution state nuclear magnetic resonanace (NMR) analysis is discussed and presented. Statistical analysis showed that there is a relationship between a targeted precision and practical pulse intervals. The bandwidth of the audio filter needs to be set so that all the signals of interest fall into 80% of the centre part of the filter. When fulfilling these conditions, the relative standard deviation (RSD) of a signal area in repeated experiments can be estimated by determining the signal-to-noise ratio (SN) of a single spectrum. When the SN reached 1000, the RSD became constant with increasing SN. With such a condition, accuracy better than 1% should be obtained with quantitative NMR.