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Determination of free fatty acids in chocolate by liquid chromatography with tandem mass spectrometry
Author(s) -
Perret Daniela,
Gentili Alessandra,
Marchese Stefano,
Sergi Manuel,
Caporossi Lidia
Publication year - 2004
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1582
Subject(s) - chemistry , chromatography , degree of unsaturation , tandem mass spectrometry , electrospray , mass spectrometry , extraction (chemistry) , solid phase extraction , liquid chromatography–mass spectrometry , chloroform , analytical chemistry (journal)
This paper describes a rapid extraction method, based on a matrix solid‐phase dispersion technique using diatomaceous earth as solid support and 50:50 (v/v) chloroform/methanol as extracting solvent, that can determine 11 free fatty acids in chocolate. The extraction procedure is followed by reversed‐phase liquid chromatography/tandem mass spectrometry (LC/MS/MS) using a normal‐bore (4.6 mm i.d.) C‐18 column and an electrospray interface operating in the negative ion mode. The tandem mass spectra of selected compounds show that charge‐remote fragmentation (CRF) mechanisms are occurring; the intensities of the CRF reactions increase with the carbon number and degree of unsaturation of the fatty acids. Average recoveries, evaluated by the standard addition method, vary between 79–103%, and the estimated quantification limits are less than 153 ng/g. The proposed method has been used to analyse nine chocolate samples from various price ranges, bought from supermarkets. Copyright © 2004 John Wiley & Sons, Ltd.