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

• Published in: Journal of Chromatography A 2014-09, Vol.1361, p.117-124
• Main Authors: Lim, Hyun-Hee, Shin, Ho-Sang
• Format: Article
• Language: English
• Subjects: Acrylamide; Biological and medical sciences; d-Cysteine; Derivatization; Food industries; Foods; Fundamental and applied biological sciences. Psychology; General aspects; Liquid chromatography–tandem mass spectrometry; Methods of analysis, processing and quality control, regulation, standards
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2014.07.094

•New novel derivatization method of acrylamide with low hazard agent, cysteine.•A liquid chromatography–tandem mass spectrometric parameters were optimized.•The method to reduce solvents use in extraction.•A simple and rapid trace analytical method of acrylamide.•Highly accurate and precise analytical method of acrylamide. 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 β-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 2.0g of food sample with 6mL of methylene chloride, and the organic extract was diluted with 3mL of hexane, and then the analyte was back-extracted with 0.5mL of pure water. The derivatization of acrylamide was performed in the water extract. The best reaction conditions (3.0mg of d-cysteine, a pH 6.5, a reaction temperature of 90°C, and a heating time of 50min) 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 0.04μg/kg and 0.14μg/kg, respectively, and the inter-day relative standard deviation was less than 8% at concentrations of 20 and 100μg/kg. The method was successfully applied to determine the amount of acrylamide in potato chips, French fries, and coffee.