Rapid sample preparation method for LC-MS/MS or GC-MS analysis of acrylamide in various food matrices

被引:147
作者
Mastovska, Katerina [1 ]
Lehotay, Steven J. [1 ]
机构
[1] USDA ARS, Eastern Reg Res Ctr, Wyndmoor, PA 19038 USA
关键词
acrylamide; sample preparation; liquid chromatography-mass spectrometry; gas chromatography-mass spectrometry; direct sample introduction;
D O I
10.1021/jf061330r
中图分类号
S [农业科学];
学科分类号
09 ;
摘要
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.
引用
收藏
页码:7001 / 7008
页数:8
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