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

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

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2011-02-01)
Ho-Sang Shin, Hyun-Hee Lim
ABSTRACT

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 β-glucuronidase/arylsulfatase was achieved with a liquid extraction using 5 mL of pentane. After addition of 50 μL 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 °C. The accuracies were in the range of 96-109% at a concentration of 0.5, 10 and 25 μg/L and their precisions were less than 15%. Method detection limits of 2-NAP and 1-HOP were 0.07 and 0.01 μg/L, respectively. This method was used to analyze twenty urine samples, and they were found in the concentration range <0.07-13.7 μg/L (2-NAP) and <0.01-0.88 μg/L (1-HOP). The concentrations of 2-NAP and 1-HOP were well correlated to those of naphthalene and pyrene in blood, respectively.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide, >97%
Supelco
MTBSTFA (with 1% t-BDMCS), (with 1% t-BDMCS), ampule of 5 × 1 mL, analytical standard, Cerilliant®
Sigma-Aldrich
N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide with 1% tert-Butyldimethylchlorosilane, ≥95%