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Untargeted Liquid Chromatography-Mass Spectrometry-Based Metabolomics Analysis of Wheat Grain
Published on: March 13, 2020
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An alternative method based on enzymatic fat hydrolysis to quantify volatile compounds in wheat bread crumb
Joana Pico1, María Jesús Nozal1, Manuel Gómez2
1I.U. Cinquima, Analytical Chemistry Group, University of Valladolid, E-47011 Valladolid, Spain.
Food Chemistry
|April 5, 2016
Summary
This study introduces a novel method for quantifying volatile compounds in wheat bread. By using lipases during extraction, the technique effectively removes fat residues, improving chromatographic analysis and accuracy.
Area of Science:
- Food Chemistry
- Analytical Chemistry
- Chromatography
Background:
- Quantifying volatile compounds in food matrices like wheat bread is crucial for understanding flavor profiles.
- Traditional methods often face challenges with fat residues interfering with chromatographic analysis.
- Existing techniques may suffer from injector contamination, column clogging, and overlapping peaks.
Purpose of the Study:
- To develop and validate an alternative, robust method for quantifying 40 volatile compounds in wheat bread crumb.
- To address and overcome the limitations posed by fat content in chromatographic analysis of bread volatiles.
- To introduce the novel use of lipases in the extraction process for improved analytical performance.
Main Methods:
- Employed Soxhlet extraction using a dichloromethane and diethyl ether solvent mixture.
- Incorporated lipases into the extraction mixture to enzymatically transform fats into free fatty acids and glycerol.
- Utilized a Vigreux column for concentration and Gas Chromatography-Mass Spectrometry (GC/MS) for analysis, with standard addition to correct matrix effects.
Main Results:
- Achieved high extraction efficiencies ranging from 70% to 100%.
- Demonstrated excellent precision with relative standard deviation (RSD) values below 15%.
- Successfully applied the method to a commercial wheat bread sample, identifying acetoin, phenylethyl alcohol, and acetic acid as major volatile compounds.
Conclusions:
- The proposed method offers a significant improvement for the analysis of volatile compounds in wheat bread crumb.
- The enzymatic fat transformation effectively prevents chromatographic interferences, leading to cleaner and more accurate results.
- This validated technique provides a reliable tool for identifying and quantifying key volatile compounds contributing to bread aroma.

