Evaluation of expanded graphite as on-line solid-phase extraction sorbent for high performance liquid chromatographic determination of trace levels of DDTs in water samples

Abstract

Dichlorodiphenyltrichloroethane (DDT) and its metabolites are a typical kind of persistent organic pollutants (POPs). Development of a simple, cost-effective and sensitive methodology to monitor DDTs concentrations in water environment is of particular significance for understanding the fate and behavior of these pollutants. In this paper, a method on the basis of solid-phase extraction (SPE) using expanded graphite (EG) as sorbent coupled on-line with high performance liquid chromatography (HPLC) was developed for the determination of trace levels of p, p′-DDD (2,2-bis(4-chlorophenyl)-1,1-dichloroethane), p, p′-DDT, o, p′-DDT and p, p′-DDE (2,2-bis(4-chlorophenyl)-1,1-dichloroethene) in water. The analytes in water were preconcentrated onto the SPE column packed with expanded graphite, and subsequently eluted with methanol–water (90:10) mixed solvent. HPLC with a photodiode array detector was used for their separation and detection. The developed on-line solid-phase extraction protocol for HPLC permits the current HPLC separation and the next preconcentration proceeded in parallel, and thus allows one determination within 8 min. The precision (R.S.D.) for 10 replicate injections of a mixture of 1 μg l −1 of each analyte was 3.2–6.2% for the peak area measurement. The detection limits (S/N = 3) for preconcentrating 50 ml of sample solution ranged from 10 to 25 ng l −1 at a sample throughput of 7.5 samples h −1. The enhancement factors were about 700. The method was applied to the determination of trace p, p′-DDD, p, p′-DDT, o, p′-DDT and p, p′-DDE in local lake, river and tap water samples.