title: Optimisation and validation of programmed temperature vaporization (PTV) injection in solvent vent mode for the analysis of the 15+1 EU-priority PAHs by GC-MS.
abstract: This paper presents the optimisation of a programmed temperature vaporization solvent vent (PTV-SV) injection gas chromatographic mass spectrometric (GC-MS) method for the analysis of the 15+1 EU-priority PAHs in food extracts. Three operation parameters (vent time, vent flow and vent pressure) were optimised by applying a D-optimal experimental design. Among these variables, vent time showed the highest effect on the analytical response (signal intensity) of the target PAHs. The 15+1 EU-priority PAHs were analysed in solvent solutions and in extracts of fortified sausage. In addition, blank lamb meat extracts were prepared and spiked with the target PAHs prior to GC-MS analysis. The performance of the optimised PTV-SV injection GC-MS method was scrutinised for linearity, precision, matrix effects and robustness. All parameters were found satisfactorily. Compared to PTV injection in splitless mode, the PTV-SV injection method provided an enhancement of sensitivity for all target PAHs. Especially significant was the improvement of the S/N ratios of the compounds with the highest molecular mass.
authors.affiliation: European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Geel, Belgium.
authors.forename: José Angel
authors.initials: JA
authors.lastname: Gómez-Ruiz
authors.forename: Fernando
authors.initials: F
authors.lastname: Cordeiro
authors.forename: Patricia
authors.initials: P
authors.lastname: López
authors.forename: Thomas
authors.initials: T
authors.lastname: Wenzl
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods*; D015394:Molecular Structure; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry*; D013696:Temperature; D014835:Volatilization
chemical_list: D011084:Polycyclic Aromatic Hydrocarbons; D012997:Solvents