Bringmann G, Wohlfarth M, Heubes M
Institute of Organic Chemistry, University of Würzburg, Germany.
J Chromatogr A. 2000 Dec 29;904(2):243-9. doi: 10.1016/s0021-9673(00)00926-2.
The first high-performance liquid chromatography-nuclear magnetic resonance (HPLC-NMR) investigation of exchangeable protons of low-molecular-mass natural products is reported. Model alkaloids or crude plant extracts were dissolved in 2H2O-1H2O-MeCN (deuterium oxide-water-acetonitrile) or 2H2O-MeCN and, after direct injection or chromatographic separation, examined in a 60-microl NMR flow probe. Exchangeable amino protons initially detected by HPLC-electrospray ionization mass spectrometry were subsequently identified and investigated by stop-flow 1H-NMR, two-dimensional (2D) total correlation spectroscopy (TOCSY), and 2D nuclear Overhauser effect spectroscopy (NOESY). These experiments extend the applicability of HPLC-NMR for the investigation and structure elucidation of natural products.
本文报道了首次对低分子质量天然产物的可交换质子进行的高效液相色谱-核磁共振（HPLC-NMR）研究。将模型生物碱或植物粗提取物溶解于2H2O-1H2O-MeCN（重水-水-乙腈）或2H2O-MeCN中，直接进样或经色谱分离后，在一个60微升的核磁共振流动探头中进行检测。最初通过HPLC-电喷雾电离质谱检测到的可交换氨基质子，随后通过停流1H-NMR、二维（2D）全相关谱（TOCSY）和二维核Overhauser效应谱（NOESY）进行鉴定和研究。这些实验扩展了HPLC-NMR在天然产物研究和结构解析方面的应用范围。
