Simultaneous Analysis of Ethylene Oxide and 2-Chloroethanol in Sesame Seeds and Other Food Commodities: Challenges and Solutions

Applications | 2022 | Agilent TechnologiesInstrumentation
GC/MSD, GC/MS/MS, GC/QQQ
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Importance of the Topic


The detection of ethylene oxide (EtO) and its metabolite 2-chloroethanol (2-CE) in sesame seeds and spices is critical due to their carcinogenic and toxic properties and strict EU maximum residue limits (MRLs). Reliable monitoring methods ensure compliance with regulations and safeguard public health.

Study Objectives and Overview


This application note presents an optimized analytical approach to simultaneously quantify EtO and 2-CE in sesame and curcuma. The method addresses challenges related to high analyte volatility, complex food matrices, instrument contamination, and chromatographic interferences.

Methodology and Instrumentation


Sample Preparation
  • QuEChERS extraction (EN 15662) with acetonitrile, water, and internal standards (EtO-D4, 2-CE-D4).
  • Dispersive SPE cleanup using PSA, C18EC, and MgSO´.

Chromatographic Analysis
  • Agilent 8890 GC with a Gerstel MPS and Automated Liner Exchange (ALEX) for cold split injection (PTV inlet).
  • Agilent 7010 Triple Quadrupole GC/MS for MRM detection.
  • Dedicated HP-VOC column and precolumn backflushing to separate EtO from acetaldehyde and remove high-boiling matrix components.

Main Results and Discussion


Chromatographic Performance
  • Baseline separation of EtO from acetaldehyde and 2-CE from matrix interferences.
  • MRM transitions optimized for high sensitivity and selectivity.

Calibration and Linearity
  • EtO linear from 5–100 ng/mL, 2-CE from 0.84–84 ng/mL (R²>0.99).

Recovery and Precision
  • Recoveries in sesame and curcuma ranged from 84.5 to 106.2% with RSD <16% across spike levels (0.05, 0.2, 0.5 mg/kg).

Instrument Robustness
  • ALEX inlet liner exchange after 20 injections prevented contamination and maintained peak shape over extended sequences.
  • Precolumn backflush protected the analytical column from nonvolatile residues.

Application to Commercial Samples
  • No EtO detected in tested retail spices, likely due to loss during storage or heat treatment.
  • 2-CE was detected in all samples, some exceeding MRLs, validating method sensitivity in real matrices.

Instrumentation Used


  • Agilent 8890 Gas Chromatograph
  • Gerstel MPS robotic sampler with Automated Liner Exchange (ALEX)
  • Agilent 7010 Triple Quadrupole GC/MS
  • HP-VOC GC column (30 m × 0.20 mm, 1.12 µm)

Benefits and Practical Applications


  • High sensitivity and selectivity allow quantification below EU MRLs.
  • Automated liner exchange and backflush minimize downtime and maintenance.
  • Adaptable to routine quality control in food and feed laboratories.

Future Trends and Applications


Further automation of sample preparation, integration with high-resolution MS, expansion to a wider range of food matrices, and incorporation of data-analysis software for rapid decision support are expected to enhance surveillance of EtO and 2-CE in the food supply.

Conclusion


This optimized QuEChERS–GC/MS/MS method meets EU requirements for EtO and 2-CE analysis in sesame and spices. It offers robust performance, low detection limits, and operational efficiencies through automated inlet maintenance and matrix protection.

Reference


1. Tateo F.; Bononi M. Journal of Food Composition and Analysis 2006, 19, 83–87.
2. Regulation (EU) 2015/868. Off. J. Eur. Union L.145, 1–71.
3. Regulation (EC) No 149/2008. Off. J. Eur. Union L.58, 1–398.
4. EURL-SRM Analytical Observation Report, Dec 2020.

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