Development of a solid phase extraction protocol for the simultaneous determination of anthracene and its oxidation products in surface waters by reversed-phase HPLC

摘要

A gradient reversed-phase high performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of anthracene, anthraquinone, and 1-hydroxyanthraquinone, with photodiode array detection at 250 nm, has been developed. This method of the determination of anthracene and its oxidation products appears in the literature for the first time. The separation has been achieved on a Kromasil 100 C8 5 < mu >m 250 x 4 mm column, applying a 10 min linear gradient elution starting with 85% methanol and 15% 0.05M ammonium acetate and ending up with 95% of methanol and 5% 0.05M ammonium acetate, at a flow-rate 0.7 mL/min, using 3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine (lamotrigine) as internal standard. Calibration curves were rectilinear for 0.1 to 3.0 ng of anthracene, for 0.1 to 10.0 ng of anthraquinone, and for 0.5 to 20.0 ng of 1-hydroxyanthraquinone, when 10 < mu >L was injected. The detection limits were found to be 0.05 ng injected on-column for anthracene and anthraquinone and 0.3 ng on-column for 1-hydroxyanthraquinone. The average intra- and inter-day R.S.Ds for injection precision (in terms of peak area) were 1.95% and 3.62%, respectively. The method was applied to the analysis of river and lake waters. A protocol, combining solid phase extraction (SPE) with sonication of matrix with sorbent, was developed for enhancement of recovery. The proposed protocol was chosen among other studied, after optimization of each step. Mean recoveries were 50% for anthracene, 71% for anthraquinone, and 105% for 1-hydroxy anthraquinone.