Arid
DOI10.1080/10826070701560652
Development and validation of a HPLC-DAD method for determination of several endocrine disrupting compounds in estuarine water
Ribeiro, Claudia; Tiritan, Maria Elizabeth; Rocha, Eduardo; Rocha, Maria Joao
通讯作者Rocha, Maria Joao
来源期刊JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
ISSN1082-6076
出版年2007
卷号30期号:18页码:2729-2746
英文摘要

This paper presents the development and validation of an analytical procedure, which allows the simultaneous quantification of nine endocrine disrupters (EDCs) in polluted surface waters. The compounds selected for this study were the natural hormones (17 beta-estradiol and estrone), the synthetic hormone (17 alpha-ethynylestradiol), the bisphenol A, the alkylphenols (4-octylphenol and 4-nonylphenol), and the phytoestrogens (daidzein, genistein, and biochanin A). Briefly, this method consisted of the preconcentration of water samples (2 L) in 500 mg Oasis HLB cartridges, followed by a cleanup step in 1 g silica cartridges, and analysis of all EDCs by High Performance Liquid Chromatography with Diode Array Detection (HPLC-DAD). The chromatographic separation occurred in a RP-18 analytical column in a gradient mode of CH3CN : H2O (pH 2) at a flow rate of 1 mL/min. The validation parameters revealed that this method was highly specific for all assayed EDCs (. 99%), the linearity of the calibration curves, obtained either by external patronization or by fortified matrix calibration techniques, always showed a correlation higher than 0.99 and their intermediate precision and repeatability, evaluated in terms of intra and inter assays, were optimal for all EDCs (RSD, 3%). The precision and accuracy, estimated as the recovery rates that occurred during the preconcentration and the cleanup processes showed, for all EDCs, excellent results (RSD, 3% and recoveries up to 116%), and preconcentration factors (enrichment) up to 10000. The limits of detection (LOD) and quantification (LOQ) were mathematically estimated from the calibration curves. As expected, these values were different for each of the nine assayed EDCs and were higher when calculated from the addition standard calibration curves. Here, 4-octylphenol was the compound with the lowest LOD and LOQ (3.8 ng/L and 12.0 ng/L) and 17 a-ethynylestradiol the one with the highest levels for both cited parameters (18.0 ng/L and 54.5 ng/L). Finally, the performance of the method was checked with water samples from a highly polluted area in the Douro river estuary (Portugal). The field results revealed high levels of estrogens (up to 176 ng/L), bisphenol A (up to 5.1 mg/L), alkylphenols (up to 449 ng/L), and phytoestrogens (up to 74 ng/L), in accordance with the high local pollution load, and suggested that this method can be easily and successfully used in water monitoring surveys of, at least, highly polluted estuarine areas.


类型Article
语种英语
国家Portugal
收录类别SCI-E
WOS记录号WOS:000250551500006
WOS关键词AQUATIC ENVIRONMENT ; ESTROGENS ; CHROMATOGRAPHY ; HORMONES ; CHEMICALS
WOS类目Biochemical Research Methods ; Chemistry, Analytical
WOS研究方向Biochemistry & Molecular Biology ; Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/155167
作者单位(1)ISCS N, Dept Pharmaceut Sci, P-4585116 Gandra PRD, Portugal;(2)CIIMAR Res, Oporto, Portugal;(3)Univ Porto, Ctr Studies Chem Phytochem & Pharmacol, CEQOFFUP, P-4100 Oporto, Portugal;(4)Univ Porto, Inst Biomed Sci Abel Salzazr ICBAS, P-4100 Oporto, Portugal
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GB/T 7714
Ribeiro, Claudia,Tiritan, Maria Elizabeth,Rocha, Eduardo,et al. Development and validation of a HPLC-DAD method for determination of several endocrine disrupting compounds in estuarine water[J],2007,30(18):2729-2746.
APA Ribeiro, Claudia,Tiritan, Maria Elizabeth,Rocha, Eduardo,&Rocha, Maria Joao.(2007).Development and validation of a HPLC-DAD method for determination of several endocrine disrupting compounds in estuarine water.JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,30(18),2729-2746.
MLA Ribeiro, Claudia,et al."Development and validation of a HPLC-DAD method for determination of several endocrine disrupting compounds in estuarine water".JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES 30.18(2007):2729-2746.
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