title: Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up.
abstract: BACKGROUND
  Numerous studies have demonstrated acrylamide to be both neurotoxic and carcinogenic. At present it is widely recognised that acrylamide is mainly formed through the Maillard reaction from free asparagine and reducing sugars. The major sources of dietary acrylamide are potato products, processed cereals and coffee.
  
  
  OBJECTIVE
  To optimise and validate an analytical method for determining acrylamide in coffee by liquid chromatography and tandem mass spectrometry analysis (LC/MS/MS) using SPE clean-up.
  
  
  METHODS
  Analytical separation of acrylamide from roasted coffee was performed by liquid chromatography using a Hypercarb column followed by LC/MS/MS analysis, with 2,3,3-d3 acrylamide as an internal standard. The method was based on two purification steps: the first with hexane and Carrez solutions in order to remove of fat and to precipitate proteins, respectively; and the second with a solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences.
  
  
  RESULTS
  Limit of quantification (LOQ) for measuring acrylamide in coffee was 50 microg/kg. The described method demonstrates satisfactory precision (RSD = 2.5%), repeatability (RSD = 9.2%) and accuracy (mean recovery - 97.4%).
  
  
  CONCLUSIONS
  Our results confirm that LC-MS/MS with SPE clean-up is selective and suitable for determination of acrylamide in coffee. Indeed, this method meets the criteria of EU Commission Recommendations (No. 2007/331/EC and No. 2010/307/EU), on the monitoring of acrylamide levels in food.
authors.affiliation: Department of Food and Food Supplements, National Food and Nutrition Institute, Warsaw, Poland. gielecin@izz.waw.pl
authors.forename: Iwona
authors.initials: I
authors.lastname: Gielecińska
authors.forename: Hanna
authors.initials: H
authors.lastname: Mojska
mesh_terms: D020106:Acrylamide / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003069:Coffee / Q000737:chemistry*; D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis; D006801:Humans; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D003069:Coffee; D020106:Acrylamide