Simultaneous Analysis of Mono‐, Di‐, Triacylglycerols, and Fatty Acid Methyl Esters in Biodiesel by Size‐Exclusion Chromatography

The purpose of this study is to develop and validate a method based on size‐exclusion chromatography (SEC) for the simultaneous determination of fatty acid methyl esters (FAME), monoacylglycerols (MAG), diacylglycerols (DAG), and triacylglycerols (TAG) in biodiesel. The proposed method presents good...

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Bibliographic Details
Published in:European journal of lipid science and technology Vol. 123; no. 12
Main Authors: da Costa, Roberta Perroni Marouço, Souza, Cristiane Gimenes, dos Santos, Rafael Cavalcante, Andrade, Débora França, Antonio d'Avila, Luiz
Format: Journal Article
Language:English
Published: Weinheim Wiley Subscription Services, Inc 01-12-2021
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Summary:The purpose of this study is to develop and validate a method based on size‐exclusion chromatography (SEC) for the simultaneous determination of fatty acid methyl esters (FAME), monoacylglycerols (MAG), diacylglycerols (DAG), and triacylglycerols (TAG) in biodiesel. The proposed method presents good linearity. The limits of detection are 0.26% mass for FAME, 0.02% mass for MAG, 0.01% mass for DAG, and 0.02% mass for TAG. The limits of quantification are 0.78% mass for FAME, 0.06% mass for MAG, 0.01% mass for DAG, and 0.06% mass for TAG. Accuracy evaluated by recovery yielded values ranging from 98.93% to 117.67%. Precision is evaluated by repeatability (%), which is ranged from 0.03% to 13.67%. The proposed SEC method proves effective in determining the FAME, MAG, DAG, and TAG content of standard samples, and the paired t‐test shows that the results obtained were statistically similar to the gas chromatography (GC) values. The method also has some advantages over the reference GC methods, since it obtains the content for each class analyzed, irrespective of its components. Also, it does not require derivatization, which makes it easier and also quicker (15 min) than the 60 min taken by the two reference methods, and it does not need an internal standard, which makes it cheaper. Practical Applications: Size exclusion chromatography (SEC) is an efficient method for simultaneous and quantitative determination of fatty acid methyl esters (FAME), monoacylglycerols (MAG), diacylglycerols and triacylglycerols (TAG). The method present itself as an alternative to reference methods (ASTM D 6584 and ABNT NBR 15764) based on gas chromatography (GC). The proposed method shows advantages compared to reference methods, once it makes possible to determine the content of each constituent class in samples, regardless of its components, what makes the peak integration easier. Beyond that, previous sample derivatization is unnecessary, what makes the method simpler, cheaper and faster (15 min) than both reference methods that demands together 60 min for analysis (ASTM D 6584 for MAG, DAGa and TAG and ABNT NBR 15764 for FAME analysis). Size‐exclusion chromatography (SEC) can be used to separate out triacylglycerols (TAG), diacylglycerols (DAG), monoacylglycerols (MAG), and fatty acid methyl esters, whose levels are specified in biodiesel. The chromatogram shows the separation of the molecules of each class according to the size of their chains. The largest molecules (TAG) are eluted first, followed by the DAG, FAME, and finally the MAG.
ISSN:1438-7697
1438-9312
DOI:10.1002/ejlt.202100069