title: Directly suspended droplet microextraction with in injection-port derivatization coupled to gas chromatography-mass spectrometry for the analysis of polyphenols in herbal infusions, fruits and functional foods.
abstract: A miniaturized liquid-phase extraction procedure based on directly suspended droplet microextraction is proposed for determining different classes of polyphenols. A derivatization reaction by means of in injection-port reaction with bis(trimethylsilyl)trifluoroacetamide is carried out to convert the polar non-volatile polyphenols into volatile derivatives. The separation and detection is carried out by coupling gas chromatography with mass spectrometry in the selected ion monitoring mode. The procedure uses undecanone, a low density organic solvent, and several factors influencing the extraction, collection efficiency and derivatization reaction are optimized. Excellent linearity was obtained for the range studied (0.05-500ngmL(-1)). The limits of detection are between 0.011 and 0.13ngmL(-1), depending on the compound, and the limits of quantification between 0.037 and 0.43ngmL(-1). The sensitivity and detection limits for polyphenols using the DSDME sample pretreatment method were very low. Enrichment factors are between 413 and 578. The recoveries obtained for spiked samples are satisfactory for all the compounds. The coupled miniaturized method is applied to the sensitive determination of both cis- and trans-resveratrol isomers, piceatannol, catechin, epicatechin, quercetin and fisetin in herbal infusions, fruits, juices and functional foods.
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia, Spain.
authors.forename: Pilar
authors.initials: P
authors.lastname: Viñas
authors.forename: Nelson
authors.initials: N
authors.lastname: Martínez-Castillo
authors.forename: Natalia
authors.initials: N
authors.lastname: Campillo
authors.forename: Manuel
authors.initials: M
authors.lastname: Hernández-Córdoba
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D005419:Flavonoids / Q000032:analysis* / Q000737:chemistry; D005638:Fruit / Q000737:chemistry; D055951:Functional Food / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D007536:Isomerism; D016014:Linear Models; D010636:Phenols / Q000032:analysis* / Q000737:chemistry; D012680:Sensitivity and Specificity; D012965:Sodium Chloride; D013662:Tea / Q000737:chemistry; D013696:Temperature; D013997:Time Factors
chemical_list: D005419:Flavonoids; D010636:Phenols; D013662:Tea; D012965:Sodium Chloride