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Glycidyl fatty acid esters in food by LC-MS/MS: method development.
A Becalski1, S Y Feng, B P-Y Lau
1Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch, Health Canada, Ottawa, Ontario, Canada. adam.becalski@hc-sc.gc.ca
Analytical and Bioanalytical Chemistry
|March 31, 2012
Summary
A new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method with stable isotope dilution analysis (SIDA) accurately quantifies glycidyl fatty acid esters in oils. This improved technique offers lower detection limits for enhanced food safety analysis.
Area of Science:
- Analytical Chemistry
- Food Chemistry
- Mass Spectrometry
Background:
- Glycidyl fatty acid esters (GE) are process contaminants found in refined edible oils and fats.
- Accurate quantification of GE is crucial for food safety regulations and risk assessment.
- Existing analytical methods may lack sensitivity or specificity for reliable GE determination.
Purpose of the Study:
- To develop and validate an improved analytical method for quantifying five key glycidyl fatty acid esters in edible oils.
- To incorporate stable isotope dilution analysis (SIDA) for enhanced accuracy and precision.
- To achieve lower method detection limits compared to previously published methods.
Main Methods:
- Liquid chromatography-tandem mass spectrometry (LC-MS/MS) with positive ion atmospheric pressure chemical ionization.
- Stable isotope dilution analysis (SIDA) using deuterium-labeled internal standards.
- Two-step solid-phase extraction (SPE) cleanup using C18 and silica cartridges.
- Analysis of glycidyl esters of palmitic, stearic, oleic, linoleic, and linolenic acids.
Main Results:
- The developed LC-MS/MS method demonstrated high sensitivity, with detection limits as low as 1-3 μg/kg when using a 0.5 g oil sample.
- Average recoveries for the five target glycidyl esters ranged from 84% to 108%.
- The method achieved detection limits 5-10 times lower than published methods, particularly when using larger sample sizes.
Conclusions:
- The developed LC-MS/MS method with SIDA provides a sensitive, specific, and accurate approach for glycidyl fatty acid ester analysis in oils.
- This method enables more reliable monitoring of GE levels in food products, contributing to improved food safety.
- The technique is suitable for routine analysis and surveys of GE in the food industry.

