title: On-line preconcentration of trace carcinogenic polycyclic aromatic hydrocarbons (PAHs) in microcolumn liquid chromatography via large volume injection.
abstract: The ability and efficiency of micro precolumns made of C30 particles, monolithic silica C18 stationary phase and quartz wool coated with C30, which act as novel solid phase absorbing materials, for the on-line enrichment of aqueous polycyclic aromatic hydrocarbons (PAHs) in microcolumn liquid chromatography (LC) was investigated. The enrichment unit was designed in such a way that micro precolumns were directly connected to a 6-port micro injection valve via fused-silica tubing (0.05 mm I.D.) in order to minimize band broadening of the samples, and the enrichment efficiency of the three materials was tested using 14 PAHs, which are selected by the US Environmental Protection Agency (US EPA), as the analytes. The separation of PAHs was evaluated by using laboratory-made C30 or ODS capillary columns and the results were compared. There were no significant differences showed from the separation of PAHs in terms of peak signal between the C30 and ODS capillary columns, but the C30 capillary column was chosen for the following experiment due to its ability to produce better repeatability than the ODS column. By using the three kinds of precolumn materials, results showed that the precolumn packed with C30 particles as well as the capillary monolithic C18 precolumns (0.1 or 0.2mm I.D.) provided better recovery than those of the quartz wool's. As long as the recovery and separation of the PAHs were concerned, 0.1mm I.D. monolithic C18 precolumn showed the best results and the R.S.D.s (N=7) for the retention time, peak area and peak height were between 0.70-1.5, 2.3-5.8 and 2.4-6.6%, respectively. Large volume injection up to 0.5 mL, i.e. 2500-fold enrichment, was possible and no negative effect on the separation profile was found. The LOD (S/N=3) were between 0.10 and 4.6 pg mL(-1), while the LOQ (S/N=10) were in the range of 0.32-15 pg mL(-1), which showed that the system is comparable to many major analytical techniques and is sensitive enough for the trace analysis of PAHs in environmental samples. The system was then applied to the determination of trace PAHs present in soil sample which was randomly taken from a nearby highway.
authors.affiliation: Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan. leewahlim@apchem.gifu-u.ac.jp
authors.forename: Lee Wah
authors.initials: LW
authors.lastname: Lim
authors.forename: Yuki
authors.initials: Y
authors.lastname: Okouchi
authors.forename: Toyohide
authors.initials: T
authors.lastname: Takeuchi