title: Assessment of robustness on analysis using headspace solid-phase microextraction and comprehensive two-dimensional gas chromatography through experimental designs.
abstract: Plackett-Burman experimental design was applied for the robustness assessment of GC×GC-qMS (Comprehensive Two-Dimensional Gas Chromatography with Fast Quadrupolar Mass Spectrometric Detection) in quantitative and qualitative analysis of volatiles compounds from chocolate samples isolated by headspace solid-phase microextraction (HS-SPME). The influence of small changes around the nominal level of six factors deemed as important on peak areas (carrier gas flow rate, modulation period, temperature of ionic source, MS photomultiplier power, injector temperature and interface temperature) and of four factors considered as potentially influential on spectral quality (minimum and maximum limits of the scanned mass ranges, ions source temperature and photomultiplier power). The analytes selected for the study were 2,3,5-trimethylpyrazine, 2-octanone, octanal, 2-pentyl-furan, 2,3,5,6-tetramethylpyrazine, and 2-nonanone e nonanal. The factors pointed out as important on the robustness of the system were photomultiplier power for quantitative analysis and lower limit of mass scanning range for qualitative analysis.
authors.affiliation: Institute of Chemistry, State University of Campinas (Unicamp), CP 6194, 13084-971 Campinas, São Paulo, Brazil.
authors.forename: Luciana F
authors.initials: LF
authors.lastname: Oliveira
authors.affiliation: Institute of Chemistry, State University of Campinas (Unicamp), CP 6194, 13084-971 Campinas, São Paulo, Brazil.
authors.forename: Soraia C G N
authors.initials: SC
authors.lastname: Braga
authors.affiliation: Institute of Chemistry, State University of Campinas (Unicamp), CP 6194, 13084-971 Campinas, São Paulo, Brazil.
authors.forename: Paulo R
authors.initials: PR
authors.lastname: Filgueiras
authors.affiliation: Institute of Chemistry, State University of Campinas (Unicamp), CP 6194, 13084-971 Campinas, São Paulo, Brazil.
authors.forename: Fabio
authors.initials: F
authors.lastname: Augusto
authors.affiliation: Institute of Chemistry, State University of Campinas (Unicamp), CP 6194, 13084-971 Campinas, São Paulo, Brazil. Electronic address: ronei@iqm.unicamp.br.
authors.forename: Ronei J
authors.initials: RJ
authors.lastname: Poppi
keywords: Chocolate; Comprehensive two-dimensional gas chromatography; Plackett–Burman design; Robustness; Volatiles