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Environmental Engineering Research 2007;12(3): 93-100. DOI: https://doi.org/10.4491/eer.2007.12.3.093
SENSITIVE DETERMINATION OF ELEVEN PHENOLIC ENDOCRINE-DISRUPTING CHEMICALS IN HUMAN URINE USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY-SELECTED ION MONITORING
Hyub Kim1, and Cheol-Hyeon Jang2
1Department of Chemistry, Pohang University of Science and Technology, Pohang 790-784, Korea
2Department of Environmental Engineering, Hanbat National University, Daejeon 305-719, Korea
Corresponding Author: Hyub Kim ,Tel: +82-54-279-8158, Fax: +82-54-279-3399, Email: khlyj@postech.ac.kr
Received: March 7, 2007;  Accepted: June 6, 2007.
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ABSTRACT
I improved an analytical method for determining trace amounts of eleven phenolic endocrinedisrupting chemicals (11 phenolic EDCs) in human urine. The 11 phenolic EDCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were 91.2~125.9%, the limits of quantitation (LOQ) for the 11 phenolic EDCs in the nanogram-per-milliliter range (0.025~1.000 ng/mL) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by 0.9300~0.9943. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.
Keywords: Endocrine disrupting chemicals | TBDMS | GC/MS-SIM | LOQ | Phenol
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