title: A fast and innovative microextraction technique, μSPEed, followed by ultrahigh performance liquid chromatography for the analysis of phenolic compounds in teas.
abstract: The objective of this study was to evaluate the efficiency of a promising solid phase microextraction technique, μSPEed, in the analysis of selected phenolic compounds from teas by ultrahigh performance liquid chromatography with photodiode array detection (μSPEed/UHPLC-PDA). The innovative μSPEed configuration uses 3-μm sorbent particles tightly packed in a disposable needle equipped with a pressure-driven valve to withdraw samples in a single direction. The system was operated by the electronic pipette eVol® and different parameters influencing the extraction efficiency, as the nature of sorbent, pH, loading and elution conditions, and solvents were optimized. The best extracting conditions were obtained by loading twice 100μL of tea samples through the PS/DVB-RP sorbent and eluting with 50μL of acidified MeOH 95%. The following chromatographic separation was carried out in an Acquity C18 BEH capillary column using a gradient of 0.1% FA and acetonitrile. The optimized μSPEed/UHPLC-PDA methodology is selective and specific and was properly validated for 8 phenolic compounds widely reported in different teas. Overall, an excellent analytical performance was obtained in the 0.2-20μg/L linear dynamic range (LDR), with very low limits of detection (LODs) and quantification (LOQs), ranging between 3.5-16.8ng/mL and 10.6-50.6ng/mL, respectively, high recoveries (89.3-103.3%), good precision (RSD<5%) and negligible matrix effect. The methodology was used to assess the target polyphenols concentration in several tea samples. Rutin and quercetin-3-glucoside were the most abundant phenolics in all tea samples analysed and, with exception of naringenin and cinnamic acid, which are present in high amounts in the investigated citric teas, remain phenolic compounds are present in trace levels.
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal.
authors.forename: Priscilla
authors.initials: P
authors.lastname: Porto-Figueira
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal.
authors.forename: José A
authors.initials: JA
authors.lastname: Figueira
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal. Electronic address: jamp@uma.pt.
authors.forename: Jorge A M
authors.initials: JA
authors.lastname: Pereira
authors.affiliation: CQM-UMa, Centro de Química da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal; Faculdade de Ciências Exactas e Engenharia da Universidade da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal.
authors.forename: José S
authors.initials: JS
authors.lastname: Câmara
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002934:Cinnamates / Q000032:analysis; D044950:Flavanones / Q000032:analysis; D057230:Limit of Detection; D010636:Phenols / Q000032:analysis*; D059808:Polyphenols / Q000032:analysis; D011794:Quercetin / Q000031:analogs & derivatives; D012431:Rutin / Q000032:analysis; D052617:Solid Phase Microextraction / Q000379:methods*; D013662:Tea / Q000737:chemistry*; D000069459:Teas, Herbal / Q000032:analysis*
chemical_list: D002934:Cinnamates; D044950:Flavanones; D010636:Phenols; D059808:Polyphenols; D013662:Tea; D000069459:Teas, Herbal; C016527:isoquercitrin; C029010:cinnamic acid; D012431:Rutin; D011794:Quercetin; C005273:naringenin
keywords: Phenolic compounds; Tea; UHPLC-PDA; μSPEed