Schefer Alexandre B, Braumann Ulrich, Tseng Li-Hong, Spraul Manfred, Soares Marisi G, Fernandes João B, da Silva Maria F G F, Vieira Paulo C, Ferreira Antonio G
NMR Division, Bruker BioSpin GmbH, D-76287 Rheinstetten, Silberstreifen, Germany.
J Chromatogr A. 2006 Sep 22;1128(1-2):152-63. doi: 10.1016/j.chroma.2006.06.059. Epub 2006 Aug 14.
Separation and characterization of limonoids from Switenia macrophylla (Meliaceae) by HPLC-NMR technique has been described. Analyses were carried out using reversed-phase gradient HPLC elution coupled to NMR (600 MHz) spectrometer in stopped-flow mode. Separated peaks were collected into an interface unit prior to NMR measurements, which were performed with suppression of solvent signals by shaped pulses sequences. Structure elucidation of the limonoids was attained by data obtained from 1H NMR, TOCSY, gHSQC and gHMBC spectra without conventional isolation that is usually applied in natural products studies.
已描述了采用高效液相色谱-核磁共振技术从大叶桃花心木（楝科）中分离和鉴定柠檬苦素类化合物的方法。分析采用反相梯度高效液相色谱洗脱与核磁共振（600 MHz）光谱仪联用，在停流模式下进行。在进行核磁共振测量之前，将分离出的峰收集到一个接口单元中，通过整形脉冲序列抑制溶剂信号来进行测量。柠檬苦素类化合物的结构解析是通过从1H NMR、TOCSY、gHSQC和gHMBC光谱获得的数据实现的，无需天然产物研究中通常采用的常规分离方法。
