Analysis of 3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters

Importance of the Topic

3-MCPD and glycidyl esters are process-induced contaminants formed during high-temperature refining of edible oils. They pose health risks and are regulated by food safety authorities worldwide. Reliable analytical methods are essential to monitor and control their levels in food products.

Objectives and Study Overview

This application note demonstrates the use of AOAC Official Method 2018.12 with the Shimadzu GCMS-TQ8050 NX for the simultaneous quantification of 3-MCPD fatty acid esters and glycidyl fatty acid esters in edible oils. The approach aims to provide robust, accurate data for compliance and quality control purposes.

Used Instrumentation

• Gas Chromatograph–Mass Spectrometer: Shimadzu GCMS-TQ8050 NX
• Column: SH-5MS (30 m × 0.25 mm I.D., 0.25 μm film thickness)
• Injection: Split mode, split ratio 20:1
• Carrier gas: Helium at 50 cm/s linear velocity
• Oven program: 50 °C (1 min) to 300 °C at 10 °C/min, hold 3 min
• Ion source temperature: 250 °C
• Ionization: Electron Ionization (EI), SIM detection
• Mass channels: 3-MCPD: m/z 147.0, 196.0, 91.0; 3-MBPD: m/z 242.0, 147.0, 91.0

Methodology

Sample preparation follows AOAC Method 2018.12, including lipid extraction, ester cleavage, and derivatization. The derivatized samples are injected into the GC-MS system under the specified conditions. SIM mode enhances selectivity and sensitivity for each analyte.

Main Results and Discussion

The method achieved clear separation of target esters between 12.1 and 13.7 minutes retention time. Calibration curves were linear over the target range with correlation coefficients above 0.995. Limits of detection and quantification meet regulatory requirements. Recovery rates ranged from 90% to 110% with repeatability (RSD) below 5%.

Benefits and Practical Application

• High sensitivity and selectivity for monitoring food contaminants
• Compliance with AOAC and international standards
• Efficient throughput for routine quality control in food testing laboratories
• Versatile platform for analyzing similar process-induced contaminants

Future Trends and Potential Applications

Future developments may include integration with high-resolution mass spectrometry, automated sample preparation workflows, and expansion to multiplexed analysis of emerging contaminants. Advanced data processing algorithms and targeted libraries will further enhance speed and accuracy.

Conclusion

The Shimadzu GCMS-TQ8050 NX coupled with the SH-5MS column provides a robust and compliant method for simultaneous determination of 3-MCPD and glycidyl esters in edible oils, supporting regulatory compliance and ensuring food safety through precise quantification of process-related contaminants.

References

• Shimadzu Corporation. Application News 01-00289 (JP, ENG). First Edition: September 2023.