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Paper
Analyst, 2003, 128, 1033 - 1036, DOI: 10.1039/b301037f
A sensitive gas chromatographic–tandem mass spectrometric method for detection of alkylating agents in water: Application to acrylamide in drinking water, coffee and snuff
Hermes Licea Pérez and Siv Osterman-Golkar
A sensitive analytical method for the analysis of acrylamide and other electrophilic agents in water has been developed. The amino acid L-valine served as a nucleophilic trapping agent. The method was applied to the analysis of acrylamide in 0.2–1 mL samples of drinking water or Millipore-filtered water, brewed coffee, or water extracts of snuff. The reaction product, N-(2-carbamoylethyl)valine, was incubated with pentafluorophenyl isothiocyanate to give a pentafluorophenylthiohydantoin (PFPTH) derivative. This derivative was extracted with diethyl ether, separated from excess reagent and impurities by a simple extraction procedure, and analyzed by gas chromatography-tandem mass spectrometry. (2H3)Acrylamide, added before the reaction with L-valine, was used as internal standard. Acrylamide and the related compound, N-methylolacrylamide, gave the same PFPTH derivative. The concentrations of acrylamides were
0.4 nmol L–1(0.03 µg acrylamide L–1) in water, 200 to 350 nmol L–1 in brewed coffee, and 10 to 34 nmol g–1 snuff in portion bags, respectively. The precision (the coefficient of variation was 5%) and accuracy of the method were good. The detection limit was considerably lower than that of previously published methods for the analysis of acrylamide.
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