Abstract
A simple and sensitive procedure has been developed for the determination of 1-hydroxypyrene in urine as a biological marker of the effects of polycyclic aromatic hydrocarbons. After enzymatic hydrolysis for conjugate cleavage, the analyte was extracted from the matrix by liquid–liquid extraction with n-hexane, the extract was evaporated to dryness, and the analyte was derivatized with the silylating reagent N,O-bis(trimethylsilyl)trifluoroacetamide into trimethylsilyl ether at room temperature. The trimethylsilyl extract was analyzed by capillary gas chromatography with mass-selective detection. Quantitative high-precision determination was achieved with the use of the isotope-labeled 1-hydroxypyrene-d9 reference standard. No matrix effects were observed. The detection limit was 0.02 ng/mL, and the linearity range was 0.1–100 ng/mL. Relative standard deviations were 0.044 and 0.064 under the conditions of repeatability and intralaboratory precision, respectively. The percentage recovery was 96–102%.
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REFERENCES
Jongeneelen, F.J., Boss, R.P., Anizon, R.B., Theuws, J.L., and Henderson, P.T., Scand. J. Work, Environ. Health, 1986, vol. 12, p. 137.
Jurgen, J. and Albrecht, S., J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2002, vol. 778, p. 31.
Rossella, F., Campo, L., Pavanello, S., Kapka, L., Sivinska, E., and Fustinoni, S., Occup. Environ. Med., 2009, vol. 66, p. 509.
Jongeneelen, F.J., Anzion, R.B.M., and Henderson, P.T., J. Chromatogr. A, 1987, vol. 413, p. 227.
Campo, L., Rossella, F., and Fustinoni, S., J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2008, vol. 875, p. 531.
Ho-Sang Shin and Hyun-Hee Lim, J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2011, vol. 879, p. 489.
Blau, K. and Halket, J.M., Handbook of Derivates for Chromatography, New York: Wiley, 1993, 2nd ed.
Knapp, D.R., Handbook of Analytical Derivatization Reaction, New York: Wiley, 1979.
Pierce, A.E., Silylation of Organic Compounds, Rockford, IL: Pierce Chemical, 1968, p. 487.
Schummer, C., Delhomme, O., Appenzeller, B.M.R., Wennig, R., and Millet, M., Talanta, 2009, vol. 77, p. 1473.
Smagunova, A.N., Pashkova, G.V., and Belykh, L.I., Matematicheskoe planirovanie eksperimenta v metodicheskikh issledovaniyakh analiticheskoi khimii (Mathematical Design of an Experiment in Methodological Research of Analytical Chemistry), Irkutsk: Irkutsk. Gos. Univ., 2015.
Guideline on bioanalytical method validation, Europe Medicines Agency, 2011. www.ema.europa.eu/en/doc uments/scientific-guideline/guideline-bioanalytical-method-validation_en.pdf. Accessed July 21, 2011.
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Translated by V. Makhlyarchuk
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Alekseenko, A.N., Zhurba, O.M., Merinov, A.V. et al. Determination of 1-Hydroxypyrene as a Biomarker for the Effects of Polycyclic Aromatic Hydrocarbons in Urine by Chromatography–Mass Spectrometry. J Anal Chem 75, 84–89 (2020). https://doi.org/10.1134/S1061934820010025
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DOI: https://doi.org/10.1134/S1061934820010025