Rapid and sensitive HILIC-ESI-MS/MS quantitation of polar metabolites of acrylamide in human urine using column switching with an online trap column

J Agric Food Chem. 2008 Nov 12;56(21):9828-34. doi: 10.1021/jf801715f. Epub 2008 Oct 9.


The carcinogen acrylamide (AA) is formed during the processing of food. AA is metabolized to mercapturic acids, which are excreted with urine. A hydrophilic interaction liquid chromatography tandem mass spectrometry method (HILIC-MS/MS) using a zwitterionic stationary phase (Zic-HILIC) was developed and validated to quantitate the mercapturic acids of AA (AAMA) and glycidamide (GAMA), and AAMA-sulfoxide in human urine. In contrast to reversed phases, the application of Zic-HILIC resulted in efficient retention and separation of these highly polar compounds. Off-line sample workup was avoided by application of column switching with a Stability BS-C17 trap column prior to the analytical column, thus minimizing interferences with the urinary matrix. Limit of quantification values (LOQs) were 0.5 microg/L (AAMA), 2.0 microg/L (AAMA-sulfoxide), and 1.0 microg/L (GAMA) in human urine. Median concentrations in urine samples ( n = 54) of six nonsmoking human subjects were 24.0 microg/L (AAMA, 7.8-79.8 microg/L), 16.7 microg/L (AAMA-sulfoxide, 6.8-70.1 microg/L), and 3.82 microg/L (GAMA, 1.0-23.6 microg/L).

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetylcysteine / chemistry
  • Acetylcysteine / urine
  • Acrylamide / chemistry
  • Acrylamide / urine*
  • Adult
  • Chromatography, Liquid / methods*
  • Female
  • Humans
  • Male
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry / methods*
  • Young Adult


  • Acrylamide
  • Acetylcysteine