title: Considerations on the determination of the limit of detection and the limit of quantification in one-dimensional and comprehensive two-dimensional gas chromatography.
abstract: Methods based on the blank signal as proposed by IUPAC procedure and on the signal to noise ratio (S/N) as listed in the ISO-11843-1 norm for determination of the limit of detection (LOD) and quantitation (LOQ) in one-dimensional capillary gas chromatography (1D-GC) and comprehensive two-dimensional capillary gas chromatography (CG×GC) are described in detail and compared for both techniques. Flame ionization detection was applied and variables were the data acquisition frequency and, for CG×GC, also the modulation time. It has been stated that LOD and LOQ estimated according to IUPAC might be successfully used for 1D-GC-FID method. Moreover, LOD and LOQ decrease with decrease of data acquisition frequency (DAF). For GC×GC-FID, estimation of LOD by IUPAC gave poor reproducibility of results while for LOQ reproducibility was acceptable (within ±10% rel.). The LOD and LOQ determined by the S/N concept both for 1D-GC-FID and GC×GC-FID methods are ca. three times higher than those values estimated by the standard deviation of the blank. Since the distribution pattern of modulated peaks for any analyte separated by GC×GC is random and cannot be predicted, LOQ and LOD may vary within 30% for 3s modulation time. Concerning sensitivity, 1D-GC-FID at 2Hz and of GC×GC-FID at 50Hz shows a ca. 5 times enhancement of sensitivity in the modulated signal output.
authors.affiliation: Institute of Analytical Chemistry, Faculty of Chemistry and Food Technology, STU, Bratislava, Slovak Republic. Electronic address: jan.krupcik@stuba.sk.
authors.forename: Ján
authors.initials: J
authors.lastname: Krupčík
authors.affiliation: Institute of Analytical Chemistry, Faculty of Chemistry and Food Technology, STU, Bratislava, Slovak Republic.
authors.forename: Pavel
authors.initials: P
authors.lastname: Májek
authors.affiliation: Institute of Analytical Chemistry, Faculty of Chemistry and Food Technology, STU, Bratislava, Slovak Republic.
authors.forename: Roman
authors.initials: R
authors.lastname: Gorovenko
authors.affiliation: Institute of Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava, Slovak Republic.
authors.forename: Jaroslav
authors.initials: J
authors.lastname: Blaško
authors.affiliation: Institute of Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava, Slovak Republic.
authors.forename: Robert
authors.initials: R
authors.lastname: Kubinec
authors.affiliation: Research Institute for Chromatography, Kortrijk, Belgium.
authors.forename: Pat
authors.initials: P
authors.lastname: Sandra
mesh_terms: D005410:Flame Ionization / Q000379:methods*; D057230:Limit of Detection; D015203:Reproducibility of Results
keywords: Comprehensive two-dimensional gas chromatography; Limit of detection and quantitation; One-dimensional gas chromatography; Signal to noise determination; Simulation of chromatograms; Standard deviation of the blank