title: Development and validation of a matrix solid-phase dispersion method to determine acrylamide in coffee and coffee substitutes.
abstract: The present study describes the development and validation of a new method based on a matrix solid-phase dispersion (MSPD) sample preparation procedure followed by GC-MS for determination of acrylamide levels in coffee (ground coffee and brewed coffee) and coffee substitute samples. Samples were dispersed in C(18) sorbent and the mixture was further packed into a preconditioned custom-made ISOLUTE bilayered SPE column (C(18)/Multimode; 1 g + 1 g). Acrylamide was subsequently eluted with water, and then derivatized with bromine and quantified by GC-MS in SIM mode. The MSPD/GC-MS method presented a LOD of 5 microg/kg and a LOQ of 10 microg/kg. Intra and interday precisions ranged from 2% to 4% and 4% to 10%, respectively. To evaluate the performance of the method, 11 samples of ground and brewed coffee and coffee substitutes were simultaneously analyzed by the developed method and also by a previously validated method based in a liquid-extraction (LE) procedure, and the results were compared showing a high correlation between them.
authors.affiliation: REQUIMTE, Serviço de Bromatologia, Faculdade de Farmácia, Univ. do Porto, Rua Aníbal Cunha, 164, 4099-030 Porto, Portugal. cristina.md.soares@gmail.com
authors.forename: Cristina M Dias
authors.initials: CM
authors.lastname: Soares
authors.forename: Rita C
authors.initials: RC
authors.lastname: Alves
authors.forename: Susana
authors.initials: S
authors.lastname: Casal
authors.forename: M Beatriz P P
authors.initials: MB
authors.lastname: Oliveira
authors.forename: José Oliveira
authors.initials: JO
authors.lastname: Fernandes
mesh_terms: D020106:Acrylamide / Q000032:analysis* / Q000737:chemistry; D053000:Analytic Sample Preparation Methods; D001628:Beverages / Q000032:analysis*; D040503:Coffea / Q000737:chemistry; D003069:Coffee / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D015203:Reproducibility of Results; D012639:Seeds / Q000737:chemistry; D052616:Solid Phase Extraction
chemical_list: D003069:Coffee; D020106:Acrylamide