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.
MATERIAL AND 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.
TY - JOUR
T1 - Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up.
AU - Gielecińska,Iwona,
AU - Mojska,Hanna,
PY - 2013/8/31/entrez
PY - 2013/8/31/pubmed
PY - 2013/9/21/medline
SP - 85
EP - 90
JF - Roczniki Panstwowego Zakladu Higieny
JO - Rocz Panstw Zakl Hig
VL - 64
IS - 2
N2 - 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. MATERIAL AND 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.
SN - 0035-7715
UR - https://www.unboundmedicine.com/medline/citation/23987075/Optimisation_and_validation_of_the_analytical_procedure_for_the_determination_of_acrylamide_in_coffee_by_LC_MS/MS_with_SPE_clean_up_
DB - PRIME
DP - Unbound Medicine
ER -
