High-Resolution NMR Spectroscopy: An Alternative Fast Tool for Qualitative and Quantitative Analysis of Diacylglycerol (DAG) Oil
High-Resolution NMR Spectroscopy: An Alternative Fast Tool for Qualitative and Quantitative Analysis of Diacylglycerol (DAG) Oil
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DOI：
10.1007/s11746-011-1848-2
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发表时间：
2011-11-01
影响因子：
2
通讯作者：
Dais, Photis
中科院分区：
文献类型：
--
作者：
Hatzakis, Emmanuel;Agiomyrgianaki, Alexia;Dais, Photis
用多核(H-1，C-13，P-31)和多维核磁共振波谱分析了二酰基甘油(DAG)油及其酰甘油和酰基链的组成。一些梯度选择的二维核磁共振技术(TOCSY、HSQC-DEPT、HSQC-TOCSY和HMBC)有助于指定复杂的一维H-1和C-13-核磁共振谱。在几种情况下，前述2D-核磁共振技术为早期的指定提供了坚实的证据，该指定基于酰基链中双键的存在和相对位置引起的化学位移变化。在三个核的核磁共振谱中整合适当的信号，可以确定DAG油的组成，被发现在这种油的可接受的限度内，即1-单酰基甘油0.40-0.60%；2-单酰基甘油0.40-0.50%；1，3-二酰基甘油57-62%；1，2-二酰基甘油28-32%；三酰基甘油9-11%；饱和脂肪酸3-5%；油酸37-45%；亚油酸49-53%；亚麻酸5-6.5%；生育酚0.24-0.27%。从三个核的核磁共振谱获得的组成结果进行了比较和讨论，从重复性和易用性的角度进行了讨论。
Multinuclear (H-1, C-13, P-31) and multidimensional NMR spectroscopy was employed for the analysis of diacylglycerol (DAG) oil and the quantification of its acylglycerols and acyl chains composition. A number of gradient selected two dimensional NMR techniques (TOCSY, HSQC-DEPT, HSQC-TOCSY, and HMBC) facilitated the assignment of the complex one dimensional H-1- and C-13-NMR spectra. In several cases, the aforementioned 2D-NMR techniques offered solid proof of earlier assignments based on chemical shift changes induced by the presence and relative positions of double bonds within the acyl chains. Integration of the appropriate signals in the NMR spectra of the three nuclei allowed the determination of DAG oil composition, which was found to be within the limits accepted for this oil, namely 1-monoacylglycerols 0.40-0.60%; 2-monoacylglycerols 0.40-0.50%; 1,3-diacylglycerols 57-62%; 1,2-diacylglycerols 28-32%; triacylglycerols 9-11%; saturated fatty acids 3-5%; oleic acid 37-45%; linoleic acid 49-53%; and linolenic acid 5-6.5%; tocopherols 0.24-0.27%. The compositional results obtained from the NMR spectra of the three nuclei were compared and discussed in terms of repeatability and ease of performance.