文献类型：期刊文献

英文题名：Purification of amide alkaloids from Piper longum L. using preparative two-dimensional normal-phase liquid chromatography x reversed-phase liquid chromatography

作者：Li, Kuiyong[1];Zhu, Wenya[1];Fu, Qing[1];Ke, Yanxiong[1];Jin, Yu[1];Liang, Xinmiao[1]

机构：[1]E China Univ Sci & Technol, Sch Pharm, Minist Educ, Engn Res Ctr Pharmaceut Proc Chem, Shanghai 200237, Peoples R China

年份：2013

卷号：138

期号：11

起止页码：3313

外文期刊名：ANALYST

收录：;WOS:【SCI-EXPANDED(收录号:WOS:000318513500033)】；

基金：This work was supported by "the Fundamental Research Funds for the Central Universities", National Natural Science Funds for Distinguished Young Scholars (20825518), and National Natural Science Funds (21005028).

语种：英文

摘要：A comprehensive off-line two-dimensional liquid chromatography (2D-LC) method coupling normal phase liquid chromatography (NPLC) and reversed phase liquid chromatography (RPLC) was developed for separation and purification of amide alkaloids from Piper longum L. In the first dimension, the crude alkaloid fractions were separated in NPLC mode and 20 fractions were collected. Then fractions 5-20 were selected for further purification in RPLC mode in the second dimension. The purities of RPLC fractions with similar structures were all identified accurately by ultra performance liquid chromatography (UPLC). In total, 28 compounds with high purity were obtained and their structures were comprehensively characterized by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR) spectroscopy. The results demonstrate that this 2D NPLC x RPLC method with good orthogonality (58.3%) was effective for the preparative separation and purification of amide alkaloids from Piper longum L.