Estimation of Ethylene Oxide and Ethylene Chlorohydrin in Foodstuffs by HS-GC/MS/MS

Importance of the Topic

Contamination of foodstuffs by ethylene oxide (ETO) and its hydrolysis product ethylene chlorohydrin (ECH) poses significant health risks, including carcinogenicity. Rapid, sensitive, and routine methods are needed to ensure product safety and regulatory compliance in the food industry.

Objectives and Study Overview

This study evaluates an automated headspace GC/MS/MS approach for the direct analysis of ETO and ECH in sesame seeds and black pepper. The goals were to achieve low detection limits, minimize sample preparation, and demonstrate robustness for routine food testing.

Methodology and Instrumentation

Samples (50 mg) were placed in 20 mL headspace vials and spiked with toluene-based calibration standards to yield matrix concentrations of 5–250 ng/g. No further extraction or cleanup was performed. Key parameters included:

• Headspace sampler: Agilent CTC PAL3, incubation at 140 °C for 20 min, agitation 250 rpm
• GC system: Agilent 8890 with DB-VRX column, split ratio 10:1, oven program from 35 °C to 240 °C
• MS/MS: Agilent 7010B triple quadrupole, electron ionization, multiple reaction monitoring transitions for ETO (m/z 44>29, 44>28, 44>14) and ECH (m/z 80>31, 80>43, 82>31)

Main Results and Discussion

Calibration curves in both matrices showed excellent linearity (R² > 0.995 for ETO, > 0.998 for ECH) across six concentration levels. A limit of quantitation of 5 ng/g was demonstrated. Repeatability at 50 ng/g gave %RSDs below 1.6%. Recoveries ranged from 81% to 104% for both analytes at low and high spike levels, confirming method accuracy across different food matrices.

Benefits and Practical Applications

The headspace GC/MS/MS method eliminates time-consuming sample preparation and reduces matrix loading on the instrument, extending consumable life. Its automation and sensitivity make it ideal for:

• Quality control in production and processing facilities
• Regulatory compliance testing of spices and seeds
• High-throughput analytical laboratories

Future Trends and Potential Applications

Further integration with trap-and-enrich techniques could push detection limits below 1 ng/g. Expanding the method to other complex food matrices and coupling with high-resolution mass spectrometry may enhance selectivity and broaden target analyte scope, including newer disinfection byproducts.

Conclusion

This application demonstrates a robust, sensitive, and fully automated headspace GC/MS/MS workflow for trace analysis of ethylene oxide and ethylene chlorohydrin in foodstuffs. The method meets stringent regulatory requirements and supports efficient routine monitoring with minimal maintenance demands.

Reference

1. Zhang J.; Zhang Y. Determination of Ethylene Oxide and Ethylene Chlorohydrin in Medical Devices Using the Agilent 8890 GC and 7697A Headspace Sampler. Agilent Technologies, 2020.
2. Markes International. Fully Automated Cryogen-Free Analysis of Ethylene Oxide and 2-Chloroethanol in Contaminated Sesame Seeds Using Headspace–Trap with Multi-Step Enrichment GC–MS. Application Note 281.
3. EU Reference Laboratories for Residues of Pesticides. Analysis of Ethylene Oxide and its Metabolite 2-Chloroethanol by QuOil or QuEChERS and GC-MS/MS. Version 1.1, December 2020.