Determination of pyrrolizidine alkaloids in Senecio species by liquid chromatography/thermospray-mass spectrometry and liquid chromatography/nuclear magnetic resonance spectroscopy

被引:34
作者
Ndjoko, K
Wolfender, JL
Röder, E
Hostettmann, K [1 ]
机构
[1] Univ Lausanne, Inst Pharmacognosie & Phytochim, BEP, CH-1015 Lausanne, Switzerland
[2] Univ Bonn, Inst Pharmazeut, D-5300 Bonn, Germany
关键词
crude extracts analysis; pyrrolizidine alkaloids; Senecio vulgaris; Asteraceae; liquid chromatography/thermospray-mass; spectrometry; LC/MS; liquid chromatography/nuclear magnetic resonance spectroscopy; LC/H-1-NMR;
D O I
10.1055/s-1999-14027
中图分类号
Q94 [植物学];
学科分类号
071001 ;
摘要
A new method using direct on-line coupling between HPLC, MS and H-1-NMR was developed for the detection and identification of pyrrolizidine alkaloids (PAs) in crude extracts of Senecio species. The PAs present in the extracts were separated on a C-18 reversed-phase column with an alkaline acetonitrile-water gradient. Molecular weight information of each peak was obtained by LC/MS and specific fragments were recorded by complementary MS/MS experiments. In order to distinguish isomeric structures of PAs, complementary LC/H-1-NMR analyses were performed in both on-flow and stop-flow modes with alkaline acetonitrile-D2O and methanol-D2O as mobile phases. This approach led to the identification of the known PAs of S. vulgaris; retrorsine (1), seneciphylline (2), and senecionine (3). The method was also applied for the analysis of African Senecio species: S. mariettae and S. venosus. Retrorsine was identified as the main PA in both species. Detection of the PAs in small amounts was achieved by LC/MS. Higher amounts of extracts (mg) had to be injected to obtain good quality on-flow LC/H-1-NMR.
引用
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页码:562 / 566
页数:5
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