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United States Department of Agriculture

Agricultural Research Service

Research Project: NOVEL TECHNOLOGIES AND TECHNIQUES FOR THE DETECTION OF RESIDUES, TOXINS, AND OTHER CHEMICALS IN FOODS Title: Rapid Sample Preparation Method for Lc-Ms/ms Or Gc-Ms Analysis for Acrylamide in Various Food Matrices

Authors
item Mastovska, Katerina
item Lehotay, Steven

Submitted to: Journal of Agricultural and Food Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: July 20, 2006
Publication Date: August 18, 2006
Citation: Mastovska, K., Lehotay, S.J. 2006. Rapid sample preparation method for lc-ms/ms or gc-ms analysis for acrylamide in various food matrices. Journal of Agricultural and Food Chemistry. 54:7001-7008

Interpretive Summary: In 2002, the toxic chemical, acrylamide, was widely reported to occur in processed foods, which set off a strong reaction from the food industry, consumer groups, regulatory agencies, and scientists. There is a need for more rapid and easier methods of analysis to detect acrylamide in processed foods, and this research describes a highly advantageous analytical method for acrylamide that meets this need. The sample preparation procedure is faster, simpler, and cheaper than other current methods, and the same sample extract is compatible with liquid chromatography/tandem mass spectrometry (LC-MS/MS) or gas chromatography/mass spectrometry (GC/MS) for quantitation and identification of acrylamide at trace levels. This method, unlike other methods using GC/MS, does not require chemical derivatization of the acrylamide for detection. The expected impact from this research is that this analytical method will become the method of choice for laboratories conducting acrylamide analysis.

Technical Abstract: 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 hexane, 10 mL water, 10 mL acetonitrile, 4 g MgSO4 and 0.5 g 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 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.

Last Modified: 10/25/2014
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