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Solid-phase extraction (SPE) and liquid chromatography-mas spectrometry (LC-MS) for the determination of free fatty acids in shellfish

From National Research Council Canada

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Name affiliation
  1. National Research Council of Canada. Measurement Science and Standards
FormatText, Article
Subjectfree fatty acids; shellfish; lipid extraction; solid phase extraction; liquid chromatography–mass spectrometry
Abstract
A novel analytical protocol for the determination of free fatty acids (FFAs; saturated, monounsaturated and polyunsaturated) in shellfish using electrospray ionisation and liquid chromatography–mass spectrometry (LC–MS) is described. Total lipids were extracted from four commercially important shellfish species using chloroform-methanol in a modification of the traditionally used Bligh and Dyer method. FFAs were recovered from lipidic shellfish extracts by solid-phase extraction (SPE) on an aminopropyl-silica column using a 98:2 v/v diethyl ether (DEE)-acetic acid solution. Ether extracts containing the FFAs were evaporated and reconstituted in 70:30 v/v methanol–chloroform before analysis by LC–MS. The limits of quantification (LOQs) of the method ranged from 60 to 560 ?g g?1 wet weight depending on the different FFAs determined with selected ion monitoring (SIM). Results demonstrate that LC–MS is well suited for identification and quantification of FFAs in shellfish and negates the use of sample derivatisation required in gas chromatographic analysis.
Publication date
Terms of use
  • Crown Copyright © 2007 Published by Elsevier B.V. All rights reserved.
In
  • Journal of Chromatography A 1145, no. 1-2 (23 March 2007): 51–57.
LanguageEnglish
Peer reviewedYes
NRC numberNRCC 42614
1251
NPARC number3538322
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Record identifierb48ffdfe-32c4-4172-90b5-d7766a334552
Record created2009-03-01
Record modified2020-05-10
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