定量NMR中多种检出限评估方法的比较
收稿日期: 2021-09-02
网络出版日期: 2021-11-01
基金资助
中国科学院仪器设备功能开发技术创新项目(2017g0105)
Comparison of Different Approaches for Estimation of the Detection Limit of Quantitative NMR
Received date: 2021-09-02
Online published: 2021-11-01
在对核磁共振（Nuclear Magnetic Resonance，NMR）定量检测进行方法验证时，检出限是一项重要的指标.本文对文献中报道的校准曲线法、校准方程参数法、数学模型法、单浓度点评估法进行了系统梳理，重点介绍了这些方法的基本原理、计算公式和特点，并针对信噪比法的不足，提出了信噪比回归曲线法.采用上述五种方法计算了水溶液中甲酸钠1H NMR检测时的检出限，并讨论了采样次数对检出限的影响.在700 MHz核磁共振谱仪上，当采样次数为64时，甲酸钠的检出限在10.4~14.4 μmol/L之间.该结果为1H NMR检出限的评估提供了参考.
陈雷 , 刘红兵 , 刘惠丽 . 定量NMR中多种检出限评估方法的比较[J]. 波谱学杂志, 2022 , 39(2) : 230 -242 . DOI: 10.11938/cjmr20212944
Limit of detection (LOD), which indicates the detection ability of an analytical method, is an important parameter used in validating quantitative 1H nuclear magnetic resonance (NMR) method. Different approaches to evaluate LOD have been reported in literature, including the calibration curve approach, regression parameters-based approach, ASTM approach (proposed by American Society of Testing Materials), EPA approach (established by the United States Environmental Protection Agency) and the signal-to-noise ratio approach. In this study, systemic analyses and summaries of all mentioned approaches were given together with their principles, equations and characteristics. A novel approach based on signal-to-ratio regression curve for determining the detection limit was proposed, which can overcome weaknesses of the signal-to-noise ratio approach. The LOD of liquid-state 1H NMR method in the determination of sodium formate in aqueous solution was calculated using 5 different approaches. The influence of the number of scans on LOD was discussed. The results showed that the LOD was in the range of 10.4~14.4 μmol/L when the number of scans was 64 with 700 MHz NMR spectrometer. In conclusion, the study can provide a reference for determining the LOD of 1H quantitative NMR.
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