期刊
JOURNAL OF CHROMATOGRAPHY A
卷 971, 期 1-2, 页码 37-45出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/S0021-9673(02)01026-9
关键词
restricted access material; column-switching; environmental analysis; endocrine disruptors; alkylphenolic compounds; steroid sex hormones
A novel methodology based on column switching LC-MS, using restricted access material (RAM), for an integrated sample clean-up and analysis of endocrine disrupting compounds in sediment samples is described. The use of RAM precolumns, that combines size exclusion and reversed-phase retention mechanisms, enables fast on-line clean-up of sediment extracts and sensitive determination of alkylphenolic compounds, bisphenol A and steroid sex hormones at low ppb level (LODs=0.5-5 ng/g). Different LiChrospher ADS RAM precolumns (Merck, Germany) with C-4, C-8 and C-18, respectively, modification of inner pore surface were tested. ADS C-4 precolumns gave the best results in terms of recovery, selectivity and sensitivity, eliminating efficiently matrix components and consequently reducing ion suppression effects. Except for the most polar compounds, all compounds exhibit complete recovery with RSD from 0.87 to 15%. A complete analysis, including efficient pressurized liquid extraction (PLE) of target compounds, on-line clean-up, chromatographic separation and MS detection takes approximately 2 h, which is a significant improvement in comparison to the methods reported previously. (C) 2002 Elsevier Science B.V. All rights reserved.
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