title: Determination of pyrrolizidine alkaloids in senecio species by liquid chromatography/thermospray-mass spectrometry and liquid chromatography/nuclear magnetic resonance spectroscopy.
abstract: A new method using direct on-line coupling between HPLC, MS and (1 )H-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/ (1)H-NMR analyses were performed in both on-flow and stop-flow modes with alkaline acetonitrile-D (2)O and methanol-D (2)O as mobile phases. This approach led to the identification of the known PAs of S. vulgaris; retrorsine, seneciphylline, and senecionine. 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/ (1)H-NMR.
authors.affiliation: Institut de Pharmacognosie et Phytochimie, BEP, Université de Lausanne, Lausanne, Switzerland.
authors.forename: K
authors.initials: K
authors.lastname: Ndjoko
authors.forename: J L
authors.initials: JL
authors.lastname: Wolfender
authors.forename: E
authors.initials: E
authors.lastname: Röder
authors.forename: K
authors.initials: K
authors.lastname: Hostettmann