Quantitative quadrupolar NMR (qQNMR) using nitrogen-14 for the determination of choline in complex matrixes
Quantitative quadrupolar NMR (qQNMR) using nitrogen-14 for the determination of choline in complex matrixes
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DOI：
10.1016/j.talanta.2021.122344
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发表时间：
2021-04-01
期刊：
影响因子：
6.1
通讯作者：
Fernandez, Ignacio
中科院分区：
文献类型：
--
作者：
Belen Ruiz-Muelle, Ana;Garcia Moreno, Paula;Fernandez, Ignacio
NMR提供了选择性地激发所选核的独特潜力，以非凡的方式避免了基质效应。首次引入定量氮-14 NMR（N-14 qNMR）光谱，作为一种可靠且经过验证的方法，用于测定各种基质中的胆碱，包括藜麦谷物，速溶咖啡和食品补充剂。用扩散PGSE、NOESY和HOESY NMR研究了重酒石酸胆碱在水溶液中的离子配对。在8个浓度水平内的方法验证（从1.58到79.0 mM）提供了400 μ g/mL的检测限（1.58 mM），定量限为1000 μ g/mL（3.95 mM），良好的线性（R-2高于0.999），日内/日间精密度低于1.24%（CV），回收率为93.5%-102.5%，完全不存在基质效应。胆碱的快速和可靠的定量以及这种新方法的准确性和简单性使其在开发可能会显着影响传统分析的分析方法中非常有用。
NMR offers the unique potential to selectively excite the chosen nuclei avoiding in an extraordinary way the matrix effect. Quantitative Nitrogen-14 NMR (N-14 qNMR) spectroscopy has been introduced for the first time as a robust and validated method to determine choline in a variety of matrixes including quinoa grains, instant coffee and food supplements. A study about the ion pairing of choline bitartrate in aqueous solution by means of diffusion PGSE, NOESY and HOESY NMR have been also provided. Validation of the method within eight concentrations levels (from 1.58 to 79.0 mM) afforded a limit of detection of 400 mu g/mL (1.58 mM), a quantification limit of 1000 mu g/mL (3.95 mM), excellent linearity (R-2 higher than 0.999), intra-/inter-day precisions lower than 1.24% (CV), recoveries of 93.5%-102.5%, and complete absence of matrix effect. The fast and reliable quantification of choline together with the accuracy and simplicity of this new approach make it useful in the development of analytical procedures that could dramatically affect traditional analysis.