Cover: The MAK Collection for Occupational Health and Safety

The MAK Collection for Occupational Health and Safety

Deutsche Forschungsgemeinschaft – Ständige Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe (MAK-Kommission)

ISSN 2509-2383



4‐tert‐Octylphenol und p‐Nonylphenol – Bestimmung von 4‐tert‐Octylphenol und p‐Nonylphenol in Urin mittels LC‐MS/MS

Biomonitoring-Methode

Wolfgang Gries1
Gabriele Leng2
Katja Küpper2
Katharina Blümlein3
Susanne Gerling3
  Thomas Göen4
  Andrea Hartwig5
  MAK Commission6

1 Currenta GmbH & Co. OHG, CUR‐SEL‐ANT‐UWA, R800, 12, 47829 Uerdingen, Deutschland
2 Currenta GmbH & Co. OHG, CUR‐SEL‐SER‐GS‐BLM – Institut für Biomonitoring, Gebäude L9, 51368 Leverkusen, Deutschland
3 Fraunhofer Institut für Toxikologie und Experimentelle Medizin (ITEM), Nikolai‐Fuchs‐Straße 1, 30625 Hannover, Deutschland
4 Friedrich-Alexander-Universität Erlangen-Nürnberg, Institut und Poliklinik für Arbeits-, Sozial- und Umweltmedizin, Henkestraße 9–11, 91054 Erlangen, Deutschland
5 Institut für Angewandte Biowissenschaften, Abteilung Lebensmittelchemie und Toxikologie, Karlsruher Institut für Technologie (KIT), Adenauerring 20a, Geb. 50.41, 76131 Karlsruhe, Deutschland
6 Ständige Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe, Deutsche Forschungsgemeinschaft, Kennedyallee 40, 53175 Bonn, Deutschland

Abstract

The working group „Analyses in Biological Materials“ of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area developed and validated the presented biomonitoring method. The analytical method described hereinafter permits the selective detection of 4‐tert‐octylphenol as well as the sum of various branched p-nonylphenol isomers in urine. After adding the labelled internal standards (13C6‐4‐tert‐octylphenol and 13C6p‐nonylphenol), the samples are enzymatically hydrolysed to release the analytes from the conjugated alkylphenols. After online SPE, the analytes are separated by liquid chromatography and analysed using tandem mass spectrometry. A quantitation limit of 2 µg/l each is obtained for the analytes. Calibration standards are prepared in pooled urine and processed in the same way as the samples to be analysed.


Keywords

Alkylphenole, 4‐tert‐Octylphenol, p‐Nonylphenol, Biomonitoring, Urin, LC‐MS/MS, online‐SPE