title: Nano-liquid chromatography coupled to time-of-flight mass spectrometry for phenolic profiling: a case study in cranberry syrups.
abstract: A new method based on nano-liquid chromatography coupled to time-of-flight mass spectrometry (nano-LC-TOF-MS) using lock-mass calibration was developed to facilitate the accurate and routine characterization and quantification of phenolic compounds. Thus, it was applied to study cranberry syrups, in which, using negative ionization mode, a total of nine phenolic compounds were unequivocally identified using standards and 38 tentatively taking into account their retention time, accurate mass (errors<5 ppm) data and isotope pattern, as well as literature. Among them, 13 compounds, belonging to flavonols and iridoids conjugated with phenolic acids, were reported for first time in cranberry or cranberry based-products. The analytical method was also validated using chlorogenic acid, p-coumaric acid, (+)-catechin, (-)-epicatechin, procyanidin A2, quercetin 3-O-glucoside, quercetin 3-O-rhamnoside, quercetin, and myricetin standards. In this way, the analytical method showed adequate linearity, with R(2) above 0.99, and acceptable values of intra- and inter-day repeatability of the retention time and peak area. The detection limits and quantification were between 1.0-15.6 ng mL(-1) and 2.0-62.5 ng mL(-1), respectively. The method can be extended to characterize phenolic compounds in other food and plant matrices, and as well biological samples.
authors.affiliation: Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain.
authors.forename: María del Mar
authors.initials: Mdel M
authors.lastname: Contreras
authors.affiliation: Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain. Electronic address: darraez@ugr.es.
authors.forename: David
authors.initials: D
authors.lastname: Arráez-Román
authors.affiliation: Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain.
authors.forename: Alberto
authors.initials: A
authors.lastname: Fernández-Gutiérrez
authors.affiliation: Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain.
authors.forename: Antonio
authors.initials: A
authors.lastname: Segura-Carretero
mesh_terms: D002396:Catechols / Q000302:isolation & purification*; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D044948:Flavonols / Q000302:isolation & purification*; D062385:Hydroxybenzoates / Q000302:isolation & purification*; D039823:Iridoids / Q000302:isolation & purification*; D057230:Limit of Detection; D028321:Plant Preparations / Q000737:chemistry; D015203:Reproducibility of Results; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization; D029799:Vaccinium macrocarpon / Q000737:chemistry*
chemical_list: D002396:Catechols; D044948:Flavonols; D062385:Hydroxybenzoates; D039823:Iridoids; D028321:Plant Preparations
keywords: Cranberry; Lock-mass calibration; Miniaturization; Nano-liquid chromatography; Phenolic compounds