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Measurement of 4-nonylphenol and 4-tert-octylphenol in human urine by column-switching liquid chromatography-mass spectrometry
Authors:Koichi Inoue  Fumio Okada  Yoshihiro Yoshimura  Shun-ichiro Izumi  Hiroyuki Nakazawa
Affiliation:a Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa-ku, Tokyo 142-8501, Japan
b Saitama Prefectural Institute of Public Health, 639-1 Kamiokubo, Urawa, Saitama 338-0824, Japan
c Department of Obstetrics and Gynecology, School of Medicine, Tokai University, Bohseidai, Isehara City, Kanagawa 25-1193, Japan
Abstract:We report a method for determining 4-nonylphenol (NP) and 4-tert-octylphenol (OP) levels in human urine samples by column-switching liquid chromatography-electrospray mass spectrometry after enzymatic deglucuronidation. The method involves enzymatic deconjugation by β-glucuronidase and correction by the stable isotopically labeled internal standard, 4-(1-methyl)octylphenol-d5. The compounds were separated by reversed-phase chromatography with a C18 column, and detected by selected ion monitoring in the negative mode. After adding an internal standard to urine samples, a direct analysis was carried out. The average recoveries of OP and NP were above 85.0% with correction using the added internal standard. The quantitation limit in the urine samples was 0.3 ng ml−1. The method enables the precise determination of standards and may be applied to the detection of trace amounts of OP and NP in human urine samples.
Keywords:Nonylphenol   Octylphenol   Column-switching LC-MS   Solid-phase extraction   Urine
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