Measurement of Urinary Monohydroxy Polycyclic Aromatic Hydrocarbons Using Automated Liquid-Liquid Extraction and Gas Chromatography/Isotope Dilution High-Resolution Mass Spectrometry

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• 作者：Zheng Li ; Lovisa C. Romanoff ; Debra A. Trinidad ; Nasira Hussain ; Richard S. Jones ; Erin N. Porter ; Donald G. Patterson Jr. ; Andreas Sj&ouml ; din
• 刊名：Analytical Chemistry
• 出版年：2006
• 出版时间：August 15, 2006
• 年：2006
• 卷：78
• 期：16
• 页码：5744 - 5751
• 全文大小：228K
• 年卷期：v.78,no.16(August 15, 2006)
• ISSN：1520-6882

文摘

A method for the measurement of 24 hydroxylated polycyclic aromatic hydrocarbon metabolites (OH-PAHs) inurine has been developed. The method is based onenzymatic deconjugation, automated liquid-liquid extraction, and gas chromatography/isotope dilution high-resolution mass spectrometry after derivatization of theOH-PAHs to the trimethylsilylated derivatives. The metabolites included in the current method are formed fromeight different parent compounds. The limits of detectionwere below 7 pg/mL when using a sample size of 2 mL ofurine, except for 1- and 2-naphthols (18 and 12 pg/mL,respectively). The enzymatic deconjugation efficiency,verified by deconjugation of urine samples spiked withges/gifchars/alpha.gif" BORDER=0>-naphthyl ges/gifchars/beta2.gif" BORDER=0 ALIGN="middle">-D-glucuronide sodium salt (1-NAP-GLU) andpyrene-1-sulfate potassium salt (1-PYR-SULF), was determined to be 97% for 1-NAP-GLU conjugate and 84%for 1-PYR-SULF. The overall coefficients of variance forsix batches of quality control samples (n = 42), was 2.9-11%. Mean method recoveries of the ¹³C-labeled internalstandards were 66-72%, except for ¹³C₆-1-naphthol(46%). The throughput of this method has been determined to be 40 samples per day per analyst. This methodis currently applied to epidemiological studies, such asthe National Exposure and Nutrition Examination Survey(NHANES), to measure human exposure to PAHs.