4.5 Article

Simultaneous determination of 2-naphthol and 1-hydroxy pyrene in urine by gas chromatography-mass spectrometry

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ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2011.01.009

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GC-MS; 1-Hydroxy pyrene; 2-Naphthol; Urine; MTBDMSTFA silylation

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A gas chromatography-mass spectrometric (GC-MS) method was developed for the determination of 2-naphthol (2-NAP) and 1-hydroxypyrene (1-HOP) in human urine. Extraction from urine after the enzyme hydrolysis with beta-glucuronidase/arylsulfatase was achieved with a liquid extraction using 5 mL of pentane. After addition of 50 mu L of N-methyl-N-(tert-butyldimethylsilyl) trifluoroacetamide (MTBDMSTFA) to prevent the loss of 2-NAP during drying, the extract was completely dried and derivatized with MTBDMSTFA for 30 min at 60 degrees C. The accuracies were in the range of 96-109% at a concentration of 0.5, 10 and 25 mu g/L and their precisions were less than 15%. Method detection limits of 2-NAP and 1-HOP were 0.07 and 0.01 mu g/L, respectively. This method was used to analyze twenty urine samples, and they were found in the concentration range < 0.07-13.7 mu g/L (2-NAP) and < 0.01-0.88 mu g/L (1-HOP). The concentrations of 2-NAP and 1-HOP were well correlated to those of naphthalene and pyrene in blood, respectively. (C) 2011 Elsevier B.V. All rights reserved.

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