Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 879, Issue 1, Pages 97-112Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/S0021-9673(00)00124-2
Keywords
water analysis; derivatization; GC; environmental analysis; endocrine disruptors; carboxylic acids; phenols; hormones; methylbutyldimethyltrifluoroacetamide
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The combined gas chromatographic determination of a number of hydroxyl-group containing endocrine disrupters, including 4-octylphenol, 4-nonylphenol, 2,4-dichlorophenol, pentachlorophenol, 4-tert.-butylbenzoic acid, bisphenol-A, 17 beta-estradiol and 17 alpha-ethynylestradiol, was investigated. Derivatization, required for sensitive determination of these compounds, was carried out using N-methyl-N-(tert.-butyldimethyltrifluoroacetamide). A number of parameters affecting the derivatization reaction, like temperature, time, matrix, solvent, and amount of reagent were studied in detail. Quantitative yields were obtained for real-life extracts after optimization, but the hormones were only mono-substituted. Both solid-phase extraction (SPE) and liquid-liquid extraction were studied as extraction methods, with emphasis on SPE material and effect of pH. Recoveries and RSD for analysis of surface water samples were 58-106 and 6-16% (n=4), respectively, when using SPE, and 109-117 and 6-14% (n=6) when using Liquid-liquid extraction. The method developed allows routine analysis of surface water for traces of endocrine disrupters. The limits of detection of were 4-6 ng/l but higher for the hormones. (C) 2000 Elsevier Science B.V. All rights reserved.
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