title: Determination of alkylresorcinols and their metabolites in biological samples by gas chromatography-mass spectrometry.
abstract: High throughput GC-MS methods for quantification of alkylresorcinols (AR), biomarkers of whole grain wheat and rye intake, in plasma and adipose tissue and their metabolites in urine were developed and optimised. Alkylresorcinols in plasma (200μL) and adipose tissues (10-50mg) were extracted with diethyl ether, whereas main AR metabolites such as DHBA and DHPPA and newly identified metabolites in urine (50μL) were extracted with ethyl acetate after enzymatic deconjugation. All extracts were purified on OASIS-MAX solid phase extraction cartridges. Plasma and adipose tissue sample extracts were then derivatised with trifluoroacetic anhydride and reconstituted in undecane, whereas AR metabolites in urine samples were derivatised with BSTFA+TMCS (99:1, v/v, 100μL). Prepared samples were quantified by GC-MS (EI-SIM). Analysis of all compounds in the different matrices showed good selectivity, sensitivity, linearity, precision (<15% within and between batches), adequate recovery (75-108%), and short total run time (10-12min). The methods developed are applicable to large-scale sample sets such as epidemiological studies.
authors.affiliation: Department of Food Science, BioCenter, Swedish University of Agriculture Science, P.O. Box 7051, SE-75007 Uppsala, Sweden. Electronic address: roksana.wierzbicka@slu.se.
authors.forename: Roksana
authors.initials: R
authors.lastname: Wierzbicka
authors.affiliation: Department of Food Science, BioCenter, Swedish University of Agriculture Science, P.O. Box 7051, SE-75007 Uppsala, Sweden. Electronic address: huaxing.wu@slu.se.
authors.forename: Huaxing
authors.initials: H
authors.lastname: Wu
authors.affiliation: Department of Virology, Veterinary Research Institute, Hudcova 70, 62100 Brno, Czech Republic. Electronic address: franek@vri.cz.
authors.forename: Milan
authors.initials: M
authors.lastname: Franek
authors.affiliation: Department of Food Science, Faculty of Food and Agriculture, United Arab Emirates University, P.O. Box 17551, Al-Ain, United Arab Emirates. Electronic address: afaf.kamal@uaeu.ac.ae.
authors.forename: Afaf
authors.initials: A
authors.lastname: Kamal-Eldin
authors.affiliation: Department of Food Science, BioCenter, Swedish University of Agriculture Science, P.O. Box 7051, SE-75007 Uppsala, Sweden; Nutritional Epidemiology Unit, Institute of Environmental Medicine, Karolinska Institutet, P.O. Box 210, SE-171-77 Stockholm, Sweden. Electronic address: rikard.landberg@slu.se.
authors.forename: Rikard
authors.initials: R
authors.lastname: Landberg
mesh_terms: D000273:Adipose Tissue / Q000737:chemistry*; D000818:Animals; D015415:Biomarkers / Q000032:analysis* / Q000737:chemistry; D004032:Diet; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D016014:Linear Models; D015203:Reproducibility of Results; D012118:Resorcinols / Q000032:analysis* / Q000737:chemistry; D012680:Sensitivity and Specificity; D013552:Swine; D000067348:Whole Grains
chemical_list: D015415:Biomarkers; D012118:Resorcinols
keywords: Alkylresorcinol; Alkylresorcinols metabolites; Biomarker; Gas chromatography–mass spectrometry; Whole grain