title: Determination of Geochemically Important Sterols and Triterpenols in Sediments Using Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry (UHPLC-MS/MS).
abstract: A fast, sensitive, and selective ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method that is able to quantify geochemical biomarkers in sediment is described. A pool of 10 sterols, which can be used as biomarkers of autochthonous (cholesterol, cholestanol, brassicasterol, ergosterol), allochthonous (stigmasterol, β-sitosterol, campesterol, and stigmastanol) and anthropogenic (coprostanol and epicoprostanol) organic matter (OM), and three triterpenols (lupeol, α-amyrin, and β-amyrin) were chosen as the analytes. The method showed excellent analytical parameters, and, compared with the traditional GC-MS methods that are commonly applied for the analysis of sterols, this method requires no sample cleanup or derivatization and presents improved values for the LOD and LOQ. UHPLC can separate the diastereoisomers (epicoprostanol, coprostanol, and cholestanol) and the isomers (lupeol, α-amyrin, and β-amyrin). The method was successfully applied for the quantification of the biomarkers, and thus, it was applied to assess the OM sources and the impacts of anthropogenic activities in sediments from different environments, such as Antarctica and other Brazilian systems (Continental Shelf, São Sebastião Channel, and Santos Estuary). Unique profiles of the biomarkers were observed for the contrasting environments, and β-amyrin and cholesterol were more predominant in the Santos Estuary and Antarctica samples, respectively. The sterol ratios indicated a higher level of sewage contamination in the Santos Estuary.
authors.affiliation: †ThoMSon Mass Spectrometry Laboratory, Chemistry Institute, University of Campinas (Unicamp), 13083-970, Campinas, SP, Brazil.
authors.forename: Giovana Anceski
authors.initials: GA
authors.lastname: Bataglion
authors.affiliation: †ThoMSon Mass Spectrometry Laboratory, Chemistry Institute, University of Campinas (Unicamp), 13083-970, Campinas, SP, Brazil.
authors.forename: Eduardo
authors.initials: E
authors.lastname: Meurer
authors.affiliation: §Deparment of Oceanography, Geoscience Institute, Federal University of Bahia (UFBA), 40170-020, Salvador, BA, Brazil.
authors.forename: Ana Cecília Rizzatti
authors.initials: AC
authors.lastname: de Albergaria-Barbosa
authors.affiliation: ‡Marine Organic Chemistry Laboratory, Oceanography Institute, University of São Paulo (USP), 05508-120, São Paulo, SP, Brazil.
authors.forename: Márcia Caruso
authors.initials: MC
authors.lastname: Bícego
authors.affiliation: ‡Marine Organic Chemistry Laboratory, Oceanography Institute, University of São Paulo (USP), 05508-120, São Paulo, SP, Brazil.
authors.forename: Rolf Roland
authors.initials: RR
authors.lastname: Weber
authors.affiliation: †ThoMSon Mass Spectrometry Laboratory, Chemistry Institute, University of Campinas (Unicamp), 13083-970, Campinas, SP, Brazil.
authors.forename: Marcos Nogueira
authors.initials: MN
authors.lastname: Eberlin
mesh_terms: D002853:Chromatography, Liquid; D004784:Environmental Monitoring / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D057230:Limit of Detection; D013261:Sterols / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D013997:Time Factors; D014315:Triterpenes / Q000032:analysis*
chemical_list: D013261:Sterols; D014315:Triterpenes