Bosco M, Culeddu N, Toffanin R, Pollesello P
POLY-biós Research Centre, Area Science Park, Trieste, Italy.
Anal Biochem. 1997 Feb 1;245(1):38-47. doi: 10.1006/abio.1996.9907.
31P NMR of lipid extracts is a reproducible, rapid, and nondegradative method for qualitative and quantitative analyses of phospholipid mixtures. This analysis, however, is hampered by the instability of the solvent system commonly used for NMR spectroscopy (CHCl3/ CH3OH/H2O-EDTA). In this work we have investigated the effects of several monophasic solvent mixtures to overcome this disadvantage. Among these mixtures we have selected a solution of triethylamine, dimethylformamide, and guanidinium chloride (Et3N/DMF-GH+) as the most efficient system. In this solvent the chemical shift dispersion of the 31P signals is about four times the frequency range observed in the standard chloroform-methanol-water system. Moreover, the stability of this solvent, as a monophasic system, allows easy reproducibility of the analysis. The use of two-dimensional 1H-31P gradient-enhanced heteronuclear multiple quantum coherence experiments can further exploit the higher resolution of the signals obtained with this solvent system for the structure elucidation of known and unidentified phospholipids.
脂质提取物的31P核磁共振是一种可重复、快速且非降解性的方法，用于磷脂混合物的定性和定量分析。然而，这种分析受到核磁共振光谱常用溶剂系统（CHCl3/CH3OH/H2O-EDTA）不稳定性的阻碍。在这项工作中，我们研究了几种单相溶剂混合物的效果，以克服这一缺点。在这些混合物中，我们选择了三乙胺、二甲基甲酰胺和氯化胍（Et3N/DMF-GH+）的溶液作为最有效的系统。在这种溶剂中，31P信号的化学位移分散约为标准氯仿-甲醇-水系统中观察到的频率范围的四倍。此外，作为单相系统，这种溶剂的稳定性使得分析易于重复。使用二维1H-31P梯度增强异核多量子相干实验可以进一步利用该溶剂系统获得的信号的更高分辨率，用于已知和未知磷脂的结构解析。
