Abstract
An analytical method for the accurate determination of essential fatty acids in cereals and green vegetables is established based on isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS). In this approach, 13C-labeled fatty acids were added as internal standards to the samples prior to the sample preparation. Repeatability and reproducibility for the analyses of the essential fatty acids extracted from homogenized cereals and green vegetables were examined to validate the ID-GC/MS method. The repeatability and reproducibility were within 2% relative standard deviation. The developed method provides higher-order measurement results with the relative expanded uncertainties of 1–2% and 2–4% for cereals and green vegetables, respectively. Based on the fatty acid measurements, the developed ID-GC/MS method can be used as a candidate reference method for the quantitation of essential fatty acids in cereals and green vegetables. The developed method was also applied to analyze several commercially available products including cereal and vegetable powders.
Highlights
Lee et al Journal of Analytical Science and Technology (2020) 11:37 volatility and decrease the polarity of compounds for gas chromatography (GC) measurements, GC coupled with mass spectrometry (MS) provides the most definitive information for the identification and quantification of fatty acids.(Lee et al, 2019a; Takemoto et al, 2003; Cruz-Hernandez et al, 2013) In many cases, a single fatty acid methyl esters (FAMEs) as an internal standard is added to the sample for the quantitative analysis of fatty acids,(Takemoto et al, 2003; CruzHernandez et al, 2013) which presents limitations in an appropriate correction of recovery during the derivatization process as well as instrument sensitivity owing to the different performances of the reactions and measurements of various fatty acids
The Comité Consultatif pour la Quantité de Matière (CCQM) identified that an isotope dilution mass spectrometry (IDMS) approach has a potential to be a primary method in chemistry.(Quinn, 1997; Richter, 1997) in this study, an isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS) method is established as a higher-order reference method, in which an isotope-labeled fatty acid is used to correct the recovery and detection sensitivity of the target fatty acid during the sample preparation steps and instrumental measurements
Fatty acid analyses by ID-GC/MS Homogenized cereal and green vegetable samples, which were developed as candidate certified reference materials (CRMs) in our laboratory, were tested to determine the overall fatty acid contents in the scan mode of GC/MS
Summary
Essential fatty acids are present in various foods as metabolites and intermediates of diverse biological processes as well as the main source of energy in human beings.(Harwood, 1988; Innis, 2008; Holman, 1998; Arbuckle et al, 1994; Neuringer et al, 1984) For humans, dietary intake is the only way to obtain essential fatty acids such as α-linolenic acid (n-3 fatty acid) and linoleic acid (n-6 fatty acid).(Innis, 1991) The low intake of essential fatty acids has a negative effect on human health.(Innis, 2008; Uauy & Dangour, 2006) It is reported that n-3 fatty acid deficiency leads to decreasedCereals and vegetables are our staple foods that provide essential dietary nutrients including fatty acids. Our research laboratory at Korea Research Institute of Standards and Science as the National Metrology Institute of Korea has been developing food-matrix certified reference materials (CRMs) along with a higher-order reference method under a project of nutritional metrology program.(Lee et al, 2017; Lee et al, 2016; Lee et al, 2019b; Shin et al, 2013) The food-matrix CRMs provide certified values for the target nutrients and can be used to verify the nutrient measurements Under this program, the IDMS methods have been developed as candidate reference methods for the quantitative analysis of individual nutrients in various foods. The developed ID-GC/MS method provides higher-order metrological measurement values, which can be a candidate reference method
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