title: 9-Fluoreneacetyl-tagged, solid-phase reagent for derivatization in direct plasma injection.
abstract: We describe here a resin-based derivatization reagent, containing a 9-fluoreneacetyl tag on a controlled-pore substrate, for direct injection analysis of amphetamine in plasma. On-line, pre-column derivatization was performed by direction injection of diluted plasma sample into an sodium dodecyl sulfate-containing mobile phase. Amphetamine was trapped in the hydrophobic derivatization column and derivatized at elevated temperature by the activated solid-phase reagent. The derivatized 9-fluoreneacetyl amphetamide was separated by reversed-phase high-performance liquid chromatography with a step gradient and determined by fluorescence detection. The synthesis scheme, characterization, and optimization of the derivatization conditions for the solid-phase reagent are described. The method was evaluated by reproducibility tests and single blind spiking analysis. This solid-phase reagent combined with a surfactant containing mobile phase provided a sensitive and simple procedure for on-line derivatization in direct injection analysis of biological fluids.
authors.affiliation: Department of Chemistry, Northeastern University, Boston, MA 02115.
authors.forename: F X
authors.initials: FX
authors.lastname: Zhou
authors.forename: I S
authors.initials: IS
authors.lastname: Krull
authors.forename: B
authors.initials: B
authors.lastname: Feibush
mesh_terms: D000661:Amphetamine / Q000097:blood* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D005449:Fluorenes / Q000737:chemistry*; D005456:Fluorescent Dyes; D006801:Humans; D007202:Indicators and Reagents; D007700:Kinetics; D013696:Temperature
chemical_list: D005449:Fluorenes; D005456:Fluorescent Dyes; D007202:Indicators and Reagents; C077873:4-benzoyloxy-2-nitrophenyl 9-fluorene acetate; D000661:Amphetamine