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定量四极核磁共振(qQNMR)结合氮-14 用于复杂基质中胆碱的测定。

Quantitative quadrupolar NMR (qQNMR) using nitrogen-14 for the determination of choline in complex matrixes.

机构信息

Department of Chemistry and Physics, Research Centre CIAIMBITAL, University of Almería, Ctra. Sacramento, s/n, 04120, Almería, Spain.

Department of Chemistry and Physics, Research Centre CIAIMBITAL, University of Almería, Ctra. Sacramento, s/n, 04120, Almería, Spain.

出版信息

Talanta. 2021 Aug 1;230:122344. doi: 10.1016/j.talanta.2021.122344. Epub 2021 Mar 23.

Abstract

NMR offers the unique potential to selectively excite the chosen nuclei avoiding in an extraordinary way the matrix effect. Quantitative Nitrogen-14 NMR (N 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 μg/mL (1.58 mM), a quantification limit of 1000 μg/mL (3.95 mM), excellent linearity (R 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.

摘要

NMR 提供了独特的潜力,可以有选择地激发所选核,以非凡的方式避免基质效应。定量氮-14 NMR(N qNMR)光谱学首次被引入,作为一种强大且经过验证的方法,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。还提供了通过扩散 PGSE、NOESY 和 HOESY NMR 研究酒石酸氢胆碱在水溶液中的离子配对的研究。该方法在八个浓度水平(从 1.58 到 79.0 mM)内进行验证,提供了 400 μg/mL(1.58 mM)的检测限、1000 μg/mL(3.95 mM)的定量限、极好的线性度(R 高于 0.999)、日内/日间精密度低于 1.24%(CV)、回收率为 93.5%-102.5%,并且完全没有基质效应。该方法快速可靠地定量胆碱,同时具有准确性和简单性,因此在开发可能对传统分析产生重大影响的分析程序方面非常有用。

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