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^1^H NMR 辅助定量分析甘油和碳酸甘油酯混合物中的碳酸甘油酯。

H NMR assisted quantification of glycerol carbonate in the mixture of glycerol and glycerol carbonate.

机构信息

School of Chemistry and Biochemistry, Thapar University, Patiala 147004, India.

School of Chemistry and Biochemistry, Thapar University, Patiala 147004, India.

出版信息

Talanta. 2018 Feb 1;178:1001-1005. doi: 10.1016/j.talanta.2017.08.103. Epub 2017 Sep 1.

DOI:10.1016/j.talanta.2017.08.103
PMID:29136787
Abstract

Glycerol carbonate (GLC) is a very important chemical having a variety of application viz., green solvent in organic synthesis, an electrolyte in lithium batteries, wetting agent in cosmetics and precursor in polymer and food industry for the synthesis of 1,3-sn-diglycerides. Hence, it is vital to find out the quick and simple method for the quantification of GLC when it is synthesized via dimethyl carbonate (DMC) assisted transesterification with glycerol (GL). Present study, proposes simple, accurate and non destructive quantitative proton nuclear magnetic resonance (qHNMR) method for the determination of GLC. Based upon the study, two different equations are proposed to calculate the GLC employing the data obtained from the H NMR spectra. qHNMR results were also validated by preparing the standard mixtures of varying concentrations of GL and GLC. Further, to conform the developed method for a real application, GLC concentration was also estimated during CaO catalyzed DMC transesterification with GL. The qHNMR assisted GLC quantification were found consistent with those obtained from high-performance liquid chromatography analysis (R = 0.99).

摘要

碳酸甘油酯(GLC)是一种非常重要的化学物质,具有多种应用,例如在有机合成中作为绿色溶剂、在锂电池中作为电解质、在化妆品中作为润湿剂以及在聚合物和食品工业中作为合成 1,3- sn-二甘油酯的前体。因此,当通过碳酸二甲酯(DMC)辅助甘油(GL)酯交换合成 GLC 时,找到快速简单的定量方法非常重要。本研究提出了一种简单、准确且无损的定量质子核磁共振(qHNMR)方法来测定 GLC。基于该研究,提出了两种不同的方程,通过从 H NMR 光谱中获得的数据来计算 GLC。qHNMR 结果还通过制备不同浓度 GL 和 GLC 的标准混合物进行了验证。此外,为了确认该方法在实际应用中的适用性,还在 CaO 催化 DMC 与 GL 酯交换过程中估算了 GLC 的浓度。qHNMR 辅助 GLC 定量与高效液相色谱分析(R = 0.99)得到的结果一致。

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