title: A new derivatization approach with D-cysteine for the sensitive and simple analysis of acrylamide in foods by liquid chromatography-tandem mass spectrometry.
abstract: 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 2.0 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 (3.0mg of d-cysteine, a pH 6.5, a reaction temperature of 90°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 μg/kg and 0.14 μg/kg, respectively, and the inter-day relative standard deviation was less than 8% at concentrations of 20 and 100 μg/kg. The method was successfully applied to determine the amount of acrylamide in potato chips, French fries, and coffee.
authors.affiliation: Department of Environmental Science, Kongju National University, Kongju 314-701, Republic of Korea.
authors.forename: Hyun-Hee
authors.initials: HH
authors.lastname: Lim
authors.affiliation: Department of Environmental Education, Kongju National University, Kongju 314-701, Republic of Korea. Electronic address: hshin@kongju.ac.kr.
authors.forename: Ho-Sang
authors.initials: HS
authors.lastname: Shin
mesh_terms: D020106:Acrylamide / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003069:Coffee / Q000737:chemistry; D003545:Cysteine / Q000031:analogs & derivatives*; D005504:Food Analysis / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D011198:Solanum tuberosum / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature
chemical_list: D003069:Coffee; D020106:Acrylamide; D003545:Cysteine
keywords: Acrylamide; Derivatization; Foods; Liquid chromatography–tandem mass spectrometry; d-Cysteine