A new derivatization approach with D-cysteine for the sensitive and simple analysis of acrylamide in foods by liquid chromatography-tandem mass spectrometry

作者：Lim Hyun Hee; Shin Ho Sang^*

来源：Journal of Chromatography A, 2014, 1361: 117-124.

DOI：10.1016/j.chroma.2014.07.094

• Acrylamide
• Liquid chromatography-tandem mass spectrometry
• Foods
• D-Cysteine
• Derivatization

A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed in order to determine the amount of acrylamide in foods after derivatization with D-cysteine. The sulfhydryl group of D-cysteine was added at the beta-site double bond of acrylamide to form 2-amino-3-(3-amino-3-oxo-propyl)sulfanyl-propanoic acid. Deuterated acrylamide (acrylamide-d3) was chosen as the internal standard (IS) for analyzing the food samples. Acrylamide was extracted from 2.0 g of food sample with 6 mL of methylene chloride, and the organic extract was diluted with 3 mL of hexane, and then the analyte was back-extracted with 0.5 mL of pure water. The derivatization of acrylamide was performed in the water extract. The best reaction conditions (3.0 mg of D-cysteine, a pH 6.5, a reaction temperature of 90 degrees C, and a heating time of 50 min) were established by the variation of parameters. The formed derivative was injected into the LC-MS/MS without further extraction or purification procedures. Separation and detection were improved with the use of an ion-pairing reagent of perfluorooctanoic acid. Under the established conditions, the limits of detection and the limits of quantification were 0.04 mu g/kg and 0.14 mu g/kg, respectively, and the inter-day relative standard deviation was less than 8% at concentrations of 20 and 100 mu g/kg. The method was successfully applied to determine the amount of acrylamide in potato chips, French fries, and coffee.

• 出版日期2014-9-26