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一种经过验证的核磁共振氢谱法,用于定量测定5-羟甲基-2(5H)-呋喃酮(一种有价值的化学中间体),该中间体存在于来自科西嘉岛的亚种C叶片的二氯甲烷提取物中。

A Validated H NMR Method for the Quantitation of 5-Hydroxymethyl-2(5H)-Furanone, a Valuable Chemical Intermediate, In a Dichloromethane Extract of subsp: C Leaves from Corsica.

作者信息

Maroselli Thomas, Paoli Mathieu, Bighelli Ange

机构信息

Université de Corse-CNRS, Équipe Chimie et Biomasse, UMR 6134 SPE, Ajaccio, France.

出版信息

J Anal Methods Chem. 2022 Aug 24;2022:9580338. doi: 10.1155/2022/9580338. eCollection 2022.

Abstract

An experimental procedure using H NMR was developed and validated to quantify 5-hydroxymethyl-2(5H)-furanone, a valuable chemical synthon ((S)-enantiomer), in a dichloromethane extract of subsp. leaves. This method, using vanillin as the internal standard, exhibited a perfect linearity of measurements (  = 1) associated with very good accuracy (relative errors comprised between -1.62% and 4.25%) and precision (reproducibility 30.51 mg ± 0.4%). The limit of detection and the limit of quantitation have been measured at 0.14 mg and 0.59 mg, respectively. The experiment time is very short since a single analysis is at the minute level. 5-Hydroxymethyl-2(5H)-furanone accounted for nearly 85% in the dichloromethane extract of subsp. leaves (1.7% of the mass of fresh leaves). This plant represents an important and natural source of (S)-5-hydroxymethyl-2(5H)-furanone (main enantiomer; determined using a GC chiral analysis).

摘要

开发并验证了一种使用核磁共振氢谱(¹H NMR)的实验方法,用于定量测定亚种叶片二氯甲烷提取物中的5-羟甲基-2(5H)-呋喃酮,这是一种有价值的化学合成子((S)-对映体)。该方法以香草醛为内标,测量显示出完美的线性关系(r² = 1),具有很高的准确度(相对误差在-1.62%至4.25%之间)和精密度(重现性为30.51 mg ± 0.4)。检测限和定量限分别测定为0.14 mg和0.59 mg。由于单次分析只需几分钟,实验时间非常短。5-羟甲基-2(5H)-呋喃酮在亚种叶片的二氯甲烷提取物中占近85%(占鲜叶质量的1.7%)。这种植物是(S)-5-羟甲基-2(5H)-呋喃酮(主要对映体;使用气相色谱手性分析测定)的重要天然来源。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6464/9433289/2feca04df81f/JAMC2022-9580338.001.jpg

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