On-line two-dimensional liquid chromatography-tandem mass spectrometric determination of estrogens in sediments

The development of an on-line system for the simultaneous determination of α-estradiol, β-estradiol, estrone and 17α-ethynylestradiol in river sediments is described. The analytes were extracted from sediments by microwave-assisted extraction. A crude extract was directly analysed by a heart-cutting two dimensional high-performance liquid chromatography-ion trap-tandem mass spectrometry with an atmospheric pressure photoionization source operating in the positive mode. The method shows excellent performance in terms of accuracy, precision, and sensitivity. The accuracy of each estrogen was in the range of 98.8-107.1%. Intra-batch and inter-batch precisions were in the range of 6.2-7.0% and 8.3-9.5%, respectively. The limits of detection ranged from 90 to 250 pg g(-1). A significant reduction in the total analysis time and a reduction in sample manipulation are the main advantages of the proposed method. Finally, the method was applied on real sediment samples.