title: Quantitative determination of caffeine, formic acid, trigonelline and 5-(hydroxymethyl)furfural in soluble coffees by 1H NMR spectrometry.
abstract: A quantitative method for the determination of caffeine, formic acid, trigonelline and 5-(hydroxymethyl)furfural (5-HMF) in soluble coffees by applying the proton nuclear magnetic resonance technique ((1)H NMR) is proposed. Each of these compounds records a singlet signal at the 7.6-9.5 ppm interval of the spectrum, and its area is used to determine the concentration. 3-(Trimethylsilyl)-2,2,3,3-tetradeuteropropionic acid is added in an exact known concentration as a reference for delta=0.00 ppm and as an internal standard. The method is applied to commercial soluble coffees and satisfactorily compared with results obtained by standard methods. The limits of detection and the coefficients of variation (N=10) are, respectively, 1.32 mg/g of solid product and 4.2% for caffeine, 0.45 mg/g and 2.6% for formic acid, 0.58 mg/g and 2.4% for trigonelline, and 0.30 mg/g and 7.3% for 5-HMF. The described method is direct and no previous derivatization is needed.
authors.affiliation: University of the Basque Country, Faculty of Chemistry, Manuel Lardizabal 3, 20018 Donostia-San Sebastián, Spain.
authors.forename: Gloria
authors.initials: G
authors.lastname: del Campo
authors.forename: Iñaki
authors.initials: I
authors.lastname: Berregi
authors.forename: Raúl
authors.initials: R
authors.lastname: Caracena
authors.forename: Juan
authors.initials: J
authors.lastname: Zuriarrain
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D002110:Caffeine / Q000032:analysis*; D002138:Calibration; D003069:Coffee / Q000737:chemistry*; D005504:Food Analysis / Q000379:methods*; D005561:Formates / Q000032:analysis*; D005662:Furaldehyde / Q000031:analogs & derivatives* / Q000032:analysis; D057230:Limit of Detection; D009682:Magnetic Resonance Spectroscopy; D012995:Solubility; D012996:Solutions; D013997:Time Factors
chemical_list: D000470:Alkaloids; D003069:Coffee; D005561:Formates; D012996:Solutions; C030544:formic acid; D002110:Caffeine; C009560:trigonelline; C008046:5-hydroxymethylfurfural; D005662:Furaldehyde