期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 407, 期 13, 页码 3637-3645出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-015-8579-4
关键词
Capillary electrophoresis; Mass spectrometry; MS-MS; Undaria pinnatifida; Harmala alkaloids; Validation
资金
- CONICET [PIP-0777]
- ANPCyT in Argentina [PICT2007-00316, PICT-PRH2009-0038]
- Ministry of Education and Science in Spain [CTQ2011-27130]
The use of algae as a foodstuff is rapidly expanding worldwide from the East Asian countries, where they are also used for medical care. Harmala alkaloids (HAlk) are a family of bioactive compounds found in the extracts of some plants, including wakame (Undaria pinnatifida), an edible marine invasive algae. HAlks are based on a characteristic beta-carboline structure with at least one amino ionizable group. In this work, we report the successful separation of a mixture of six HAlks (harmine, harmaline, harmol, harmalol, harmane, and norharmane) by capillary electrophoresis ion-trap mass spectrometry (CE-IT-MS) in less than 8 min. Optimum separation in fused-silica capillaries and detection sensitivity in positive-ion mode were achieved using a background electrolyte (BGE) with 25 mmol L-1 ammonium acetate (pH 7.8) and 10 % (v/v) methanol, and a sheath liquid with 60:40 (v/v) isopropanol-water and 0.05 % (v/v) formic acid. The separation method was validated in terms of linearity, limits of detection and quantification, repeatability, and reproducibility. Later, a sample pretreatment was carefully optimized to determine HAlks in commercial wakame samples with excellent recovery and repeatability. For the complex wakame extracts, the MS-MS fragmentation patterns of the different HAlks were useful to ensure a reliable identification. The complete procedure was validated using the standard-addition calibration method, determining matrix effects on the studied compounds. Harmalol, harmine, and harmaline were naturally present in the samples and were quantified at very low concentrations, ranging from 7 to 24 mu g kg(-1) dry algae.
作者
我是这篇论文的作者
点击您的名字以认领此论文并将其添加到您的个人资料中。
推荐
暂无数据