GC/MS Identification of Flavor and Fragrance Allergens in Some Common Snack Foods Using an Agilent J&W DB-17ms Capillary GC Column

Significance of the topic

The analysis of regulated flavor and fragrance allergens in food matrices such as candy and chewing gum is critical to ensure consumer safety and compliance with European Union directives. Cinnamon-related compounds—five of the 26 EU-listed allergens—can occur at percent levels in flavored snacks, far exceeding cosmetic product limits when ingested. Reliable detection and identification of these allergens at low parts-per-million levels support quality control, regulatory compliance, and public health.

Study objectives and overview

This application evaluates a streamlined single-column GC/MS approach using an Agilent J&W DB-17ms capillary column for the separation and identification of 24 GC/MS-amenable EU flavor and fragrance allergens in candy and gum. The goal was to achieve sensitive, reproducible detection at 8 ppm—20 percent below the EU leave-on limit of 10 ppm—through a simple MTBE extraction and split injection method.

Methodology and Instrumentation

Sample preparation involved grinding snack samples, aqueous wetting, and extraction with methyl tert-butyl ether (MTBE). Extracts were analyzed by GC/MS on an Agilent 7890A GC coupled to a 5975C mass selective detector, fitted with an Agilent J&W DB-17ms 30 m × 0.25 mm, 0.25 µm column. Key parameters included a 50:1 split injection of 1 µL at 250 °C, helium carrier at 13.19 psi, and a programmed oven ramp from 150 °C to 280 °C. Calibration employed a 24-compound standard mix with internal standard 1,4-dibromobenzene at 8 ng/µL.

Main results and discussion

Repeatability tests on cinnamon gum extracts yielded a cinnamaldehyde content of 0.22 ± 0.01 wt % with 4.3 percent RSD over five replicates, demonstrating high precision of the MTBE extraction. Chromatographic resolution on the DB-17ms column allowed baseline or adequate separation of all 24 allergens at 8 ppm. Isomeric pairs such as citral, farnesol, and lyral exhibited distinct elution profiles. Real snack extracts confirmed detectable levels of key allergens—cinnamaldehyde, benzyl alcohol, eugenol, and others—at concentrations far above regulatory thresholds.

Benefits and practical applications

• Fast, single-column GC/MS workflow reduces complexity and hardware requirements compared to multi-dimensional approaches
• MTBE extraction offers simple sample preparation compatible with diverse snack matrices
• Sensitivity at 8 ppm meets or exceeds EU cosmetic leave-on limits, ensuring robust compliance monitoring
• Method supports semiquantitative screening for quality control in food production facilities

Future trends and opportunities

• Solid-phase extraction using MTBE for enhanced cleanup and matrix removal
• Capillary flow backflushing to extend column life and reduce late-eluting interferences
• Integration of deconvolution software to streamline data processing and identification
• Lower split ratios or on-column injection for improved detection limits in complex samples

Conclusion

A straightforward MTBE extraction combined with Agilent GC/MS on a DB-17ms column enables reliable identification of 24 EU-listed flavor and fragrance allergens in snack foods at low ppm levels. The method demonstrates strong repeatability and resolves critical isomeric compounds, offering a practical solution for food safety laboratories and regulatory compliance checks.

References

1. EU Directive 2003/15/EC Official Journal of the European Union 2003
2. W. Luan, C. Sandy, M. Szelewski Determination of Allergens in Fragrance Products Using Agilent Deconvolution Reporting Software Agilent Technologies publication 5989-8723EN 2008
3. F. David, M.S. Klee Analysis of Suspected Flavor and Fragrance Allergens in Perfumes Using Two-Dimensional GC with LTM Oven Module Agilent Technologies publication 5990-3576EN 2009