Rapid sample preparation method for LC-MS/MS or GC-MS analysis of acrylamide in various food matrices.
A fast and easy sample preparation procedure for analysis of acrylamide in various food matrices was developed and optimized. In its first step, deuterated acrylamide internal standard is added to 1 g of homogenized sample together with 5 mL of hexane, 10 mL of water, 10 mL of acetonitrile, 4 g of MgSO4, and 0.5 g of NaCl. Water facilitates the extraction of acrylamide; hexane serves for sample defatting; and the salt combination induces separation of water and acetonitrile layers and forces the majority of acrylamide into the acetonitrile layer. After vigorous shaking of the extraction mixture for 1 min and centrifugation, the upper hexane layer is discarded and a 1 mL aliquot of the acetonitrile extract is cleaned up by dispersive solid-phase extraction using 50 mg of primary secondary amine sorbent and 150 mg of anhydrous MgSO4. The final extract is analyzed either by liquid chromatography-tandem mass spectrometry or by gas chromatography-mass spectrometry (in positive chemical ionization mode) using the direct sample introduction technique for rugged large-volume injection.
Mastovska
Katerina
K
Eastern Regional Research Center, Agricultural Research Service, USDA, 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, USA.
Lehotay
Steven J
SJ
D020106:Acrylamide / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007202:Indicators and Reagents; D008278:Magnesium Sulfate; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity
D007202:Indicators and Reagents; D020106:Acrylamide; D008278:Magnesium Sulfate