title: Nano-liquid chromatography in nutraceutical analysis: determination of polyphenols in bee pollen.
abstract: In this study, a nano-liquid chromatography based method for the simultaneous separation of 16 polyphenols employing UV-vis detection has been developed. A 100 μm I.D. capillary column packed with C18 core-shell particles (2.6 μm particle size, 100 Å) for 10 cm was employed. The separation of analytes was performed with a step gradient in less than 20 min, using 0.5% formic acid aqueous solution and acetonitrile as eluents. The optimized analytical method was validated and the resulting RSD% for intra-day and inter-day repeatability, related to retention time, retention factor and peak area, were below 4.68 and 5.57%, respectively. LOD and LOQ values were as low as 0.78 and 3.12 μg/mL, while linearity, assessed in the concentration range of interest for all analytes, gave R(2)≥0.990. The method was finally applied to the analysis of polyphenols extracted from a collected bee pollen. Nine polyphenols, namely o-, p-coumaric acid, ferulic acid, myricetin, cinnamic acid, quercetin, naringenin, hesperitin and kaempferol, were identified. All analytes, with the exception of p-coumaric acid and myricetin, which partially co-eluted with other pollen components, were also quantified in the sample.
authors.affiliation: Centro Integrato di Ricerca, Campus Bio-Medico University, Via Alvaro del Portillo 21, 00128 Rome, Italy.
authors.forename: Chiara
authors.initials: C
authors.lastname: Fanali
authors.forename: Laura
authors.initials: L
authors.lastname: Dugo
authors.forename: Anna
authors.initials: A
authors.lastname: Rocco
mesh_terms: D000818:Animals; D001516:Bees; D002853:Chromatography, Liquid / Q000379:methods*; D003373:Coumaric Acids / Q000032:analysis; D019587:Dietary Supplements / Q000032:analysis*; D005419:Flavonoids / Q000032:analysis; D006115:Greece; D036103:Nanotechnology / Q000379:methods*; D011058:Pollen / Q000737:chemistry*; D059808:Polyphenols / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D003373:Coumaric Acids; D005419:Flavonoids; D059808:Polyphenols
keywords: Bee pollen; Core–shell stationary phase; Nano-liquid chromatography; Polyphenols