RESUMO
AIM: To identify the main metabolites of stachydrine in rat. METHODS: The ionization, cleavage and chromatographic characteristics of stachydrine were studied by using high-performance liquid chromatography-electrospray ionization ion trap tandem mass spectrometry (HPLC-ESI/MS) for the first time. These characteristics of stachydrine were used as the basis for the analyses of metabolites in rat urine. The 0 - 24 h urine samples of rats after ig 25 mg x kg(-1) stachydrine were collected and purified by using C10 solid-phase extraction cartridge, and then analyzed by HPLC-ESI/MS to identify stachydrine and its metabolites. RESULTS: The parent drug (stachydrine), 6 phase I metabolites (N-demethyl, dehydrogenation, ring-oxidation) and 2 phase II metabolites (glycine conjugates of 2 ring-oxidation products) were identified existing in rat urine. CONCLUSION: The presented method was proved to be sensitive, rapid, high selective and specific for the identification of stachydrine and its metabolites in rat urine.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Prolina/análogos & derivados , Espectrometria de Massas por Ionização por Electrospray/métodos , Stachys , Animais , Raízes de Plantas/química , Plantas Medicinais/química , Prolina/isolamento & purificação , Prolina/metabolismo , Prolina/urina , Ratos , Ratos Wistar , Sensibilidade e Especificidade , Stachys/químicaRESUMO
AIM: To establish a rapid and sensitive LC-MSn method for the identification of trigonelline and its main metabolites in rat urine. METHODS: After optimizing the detection conditions of LC-MSn chromatography and mass spectrometry using trigonelline, its ionization and cleavage in ESI-MS and ESI-MSn modes were summarized, then serving as the basis for the metabolite analysis of trigonelline in rat urine. The 0-48 h urine samples of rats were collected after iv 8 mg x kg(-1) trigonelline, then, the samples were purified through C18 solid-phase extraction cartridge. The purified samples were analyzed by LC-MSn. RESULTS: The structures of trigonelline metabolites were elucidated according to the changes of the molecular weights of the metabolites (deltaM) and their cleavage pattern in ESI-ITMSn. As a result, two phase I metabolites and the parent drug were identified existing in rat urine, and two phase II metabolites were identified. CONCLUSION: The LC-MSn method is rapid and high sensitive and specific, it is suitable for the identification of trigonelline and its metabolites in rat urine.
Assuntos
Alcaloides/metabolismo , Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Alcaloides/química , Alcaloides/isolamento & purificação , Animais , Hipoglicemiantes/química , Hipoglicemiantes/isolamento & purificação , Hipoglicemiantes/metabolismo , Masculino , Plantas Medicinais/química , Ratos , Ratos Wistar , Sensibilidade e Especificidade , Trigonella/químicaRESUMO
AIM: To estabilish a rapid and sensitive LC-ESI-ITMSn method for the identification of ephedrine and its main metabolites in rat urine. METHODS: After optimizing the detection condition of LC-ESI-ITMSn chromatography and mass spectrometry by using a standard ephedrine, the ionization and cleavage rules of ephedrine in ESI-MS and ESI-MSn modes were summarized, and then serving as the basis for the metabolite analysis of ephedrine in rat urine. Rat urine samples of 0-48 h were collected after ig 10 mg x kg(-1) ephedrine, then the samples were purified through C18 solid-phase extraction cartridge. The purified samples were analyzed by LC-ESI-ITMSn. RESULTS: The structures of ephedrine metabolites were elucidated according to the changes of the molecular weights of the metabolites (deltaM) and their cleavage pattern in ESI-ITMSn. As a result, three phase I metabolites and the parent drug ephedrine were identified existing in rat urine, but no phase II metabolites were found. CONCLUSION: The LC-ESI-ITMSn method is rapid and highly sensitive and sepecific, it is suitable for the identification of ephedrine and its metabolites in rat urine.
