title: Rapid assessment of bioactive phenolics and methylxanthines in spent coffee grounds by FT-NIR spectroscopy.
abstract: Spent coffee grounds (SCGs) are a great source of bioactive compounds with interest to pharmaceutical and cosmetic industries. Phenolics and methylxanthines are the main health related compounds present in SCG samples. Content estimation of these compounds in SCGs is of upmost importance in what concerns their profitable use by waste recovery industries. In the present work, near-infrared spectroscopy (NIRS) was proposed as a rapid and non-destructive technique to assess the content of three main phenolics (caffeic acid, (+)-catechin and chlorogenic acid) and three methylxanthines (caffeine, theobromine and theophylline) in SCG samples obtained from different coffee brands and diverse coffee machines. The content of these compounds was determined for 61 SCG samples by HPLC coupled with diode-array detection. Partial least squares (PLS) regression based models were calibrated to correlate diffuse reflectance NIR spectra against the reference data for the six parameters obtained by HPLC. Spectral wavelength selection and number of latent variables were optimized by minimizing the cross-validation error. PLS models showed good linearity with a coefficient of determination for the prediction set (Rp(2)) of 0.95, 0.92, 0.88, 071 and 0.84 for caffeine, caffeic acid, (+)-catechin, chlorogenic acid and theophylline, respectively. The range error ratio (RER) was higher for caffeine (17.8) when compared to other compounds (12.0, 10.1, 7.6 and 9.2, respectively for caffeic acid, (+)-catechin, chlorogenic acid and theophylline). Moreover, the content of caffeine could be used to predict the antioxidant properties of SCG samples (R=0.808, n=61), despite not presenting this property itself. The results obtained confirmed that NIRS is a suitable technique to screen SCG samples unveiling those with high content of bioactive compounds, which are interesting for subsequent extraction procedures.
authors.affiliation: UCIBIO, REQUIMTE, Department of Chemical Sciences, Faculty of Pharmacy, University of Porto, Rua de Jorge Viterbo Ferreira, 228, Porto 4050-313, Portugal.
authors.forename: Luís M
authors.initials: LM
authors.lastname: Magalhães
authors.affiliation: LAQV, REQUIMTE, Department of Chemical Sciences, Faculty of Pharmacy, University of Porto, Rua de Jorge Viterbo Ferreira, 228, Porto 4050-313, Portugal.
authors.forename: Sandia
authors.initials: S
authors.lastname: Machado
authors.affiliation: UCIBIO, REQUIMTE, Department of Chemical Sciences, Faculty of Pharmacy, University of Porto, Rua de Jorge Viterbo Ferreira, 228, Porto 4050-313, Portugal.
authors.forename: Marcela A
authors.initials: MA
authors.lastname: Segundo
authors.affiliation: iMed, Departamento de Farmácia Galénica e Tecnologia Farmacêutica, Faculdade de Farmácia, Universidade de Lisboa, Av. Prof. Gama Pinto, Lisbon 1649-003, Portugal.
authors.forename: João A
authors.initials: JA
authors.lastname: Lopes
authors.affiliation: LAQV, REQUIMTE, Department of Chemical Sciences, Faculty of Pharmacy, University of Porto, Rua de Jorge Viterbo Ferreira, 228, Porto 4050-313, Portugal. Electronic address: rnpascoa@ff.up.pt.
authors.forename: Ricardo N M J
authors.initials: RN
authors.lastname: Páscoa
mesh_terms: D002109:Caffeic Acids / Q000032:analysis; D002110:Caffeine / Q000032:analysis; D002392:Catechin / Q000032:analysis; D002726:Chlorogenic Acid / Q000032:analysis; D003069:Coffee / Q000737:chemistry*; D019265:Spectroscopy, Near-Infrared; D013805:Theobromine / Q000032:analysis; D013806:Theophylline / Q000032:analysis; D014866:Waste Products / Q000032:analysis*
chemical_list: D002109:Caffeic Acids; D003069:Coffee; D014866:Waste Products; D002726:Chlorogenic Acid; D002110:Caffeine; D002392:Catechin; D013806:Theophylline; D013805:Theobromine; C040048:caffeic acid
keywords: Caffeine; Chemometrics; Chlorogenic acid; Methylxanthines; Near-infrared spectroscopy; Partial least squares regression; Phenolic compounds; Spent coffee grounds