title: Injection-port derivatization coupled to GC-MS/MS for the analysis of glycosylated and non-glycosylated polyphenols in fruit samples.
abstract: Polyphenols, including glycosylated polyphenols, were analyzed via a procedure based on injection-port derivatization coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The polyphenols in lyophilized fruit samples were extracted with an acidified MeOH mixture assisted by ultrasound. Samples were dried under vacuum, and carbonyl groups were protected with methoxylamine. Free hydroxyl groups were subsequently silylated in-port. Mass fragmentations of 17 polyphenol and glycosylated polyphenol standards were examined using Multiple Reaction Monitoring (MRM) as the acquisition mode. Furthermore, in-port derivatization was optimized in terms of optimal injection port temperature, derivatization time and sample: N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) volume ratio. A C18 solid-phase-extraction clean-up method was used to reduce matrix effects and injection liner degradation. Using this clean-up method, recoveries for samples spiked at 1 and 10μg/g ranged from 52% to 98%, depending on the chemical compound. Finally, the method was applied to real fruit samples containing the target compounds. The complete chromatographic runtime was 15min, which is faster than reported for recent HPLC methods able to analyze similar compounds.
authors.affiliation: Department of Chemistry, University of Lleida and Lleida-Agrotecnio Center, Rovira Roure 191, 25198 Lleida, Spain.
authors.forename: Alexis
authors.initials: A
authors.lastname: Marsol-Vall
authors.affiliation: Department of Chemistry, University of Lleida and Lleida-Agrotecnio Center, Rovira Roure 191, 25198 Lleida, Spain. Electronic address: balcells@quimica.udl.cat.
authors.forename: Mercè
authors.initials: M
authors.lastname: Balcells
authors.affiliation: Department of Chemistry, University of Lleida and Lleida-Agrotecnio Center, Rovira Roure 191, 25198 Lleida, Spain.
authors.forename: Jordi
authors.initials: J
authors.lastname: Eras
authors.affiliation: Department of Chemistry, University of Lleida and Lleida-Agrotecnio Center, Rovira Roure 191, 25198 Lleida, Spain.
authors.forename: Ramon
authors.initials: R
authors.lastname: Canela-Garayoa
mesh_terms: D000081:Acetamides / Q000737:chemistry; D005463:Fluoroacetates / Q000737:chemistry; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006031:Glycosylation; D057230:Limit of Detection; D059808:Polyphenols / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature; D014297:Trimethylsilyl Compounds / Q000737:chemistry
chemical_list: D000081:Acetamides; D005463:Fluoroacetates; D059808:Polyphenols; D014297:Trimethylsilyl Compounds; C086665:N-methyl-N-(trimethylsilyl)trifluoroacetamide
keywords: Fruit samples; GC–MS/MS; Glycosylated polyphenols; In-port derivatization; Non-glycosylated polyphenols