Post-column in-source derivatisation in LC-MS: a tool for natural products characterisation and metabolomics.

作者: Adriana M. Cirigliano , Gabriela M. Cabrera

DOI: 10.1002/PCA.2926

关键词: AldehydeChromatographyChemistryAdductAtmospheric-pressure chemical ionizationLiquid chromatography–mass spectrometryElectrosprayPhenylhydrazineMass spectrometryNucleophilic addition

摘要: Introduction An efficient characterisation of metabolites is a crucial task in many aspects basic research, such as the de-replication crude extracts natural products chemistry or tentative identification compounds untargeted metabolomics. Objective The goal this work evaluation reaction with phenylhydrazine for derivatisation post-column situ carbonyl-containing liquid chromatography-mass spectrometry (LC-MS). Materials and methods LC-MS was performed using electrospray, Atmospheric Pressure Chemical Ionisation (APCI) Photoionization (APPI) ionisation techniques. addition done through syringe pump via T-junction before entrance to ion source. Results A variety having carbonyl groups, cycloartanes, steroids, cardenolides other terpenoids, were analysed by method. In case non-hindered aldehyde keto main signals mass spectra those corresponding phenylhydrazones. However, hindered groups displayed mainly product nucleophilic adduct carbonyl, which first step process. Finally, conjugated ketones did not react phenylhydrazine. This methodology applied analysis extracts. Conclusion results show that source achieved, yielding typical derivatives

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