Highly Selective GC/TQ Analysis of 57 Allergens in Cosmetic Products

Significance of the topic

Allergenic fragrance substances are a growing concern for consumer safety and regulatory compliance in the cosmetics industry. Recent expansions of regulatory lists, including the EU’s Regulation 2023/1545 and the US MoCRA framework, require manufacturers to detect and label a broader range of potential allergens. This drives the need for analytical methods with high selectivity and reliable quantitation to prevent false positives and negatives.

Study objectives and overview

The main objective was to develop and validate a gas chromatography–triple quadrupole mass spectrometry (GC/TQ) method for the analysis of 57 allergenic fragrance compounds and their isomers in complex cosmetic matrices. Key goals included transferring an existing GC/MSD method, improving selectivity through multiple reaction monitoring (MRM), and demonstrating robust quantitation across a relevant concentration range.

Methodology

Samples were prepared via serial dilution of standard allergen mixes. A dual-column GC configuration (polar and apolar phases) was employed to confirm compound identity and minimize coelution. The GC oven program featured an initial hold at 50 °C, ramped to 200 °C at 7 °C/min and to 240 °C at 25 °C/min, with flow maintained at 1 mL/min. The triple quadrupole MS operated in combined MRM/scan mode, with transitions optimized automatically by MassHunter Optimizer, leveraging precursor ions from the original GC/MSD method.

Used instrumentation

• Agilent 8890 gas chromatograph
• Agilent 7000E GC/TQ triple quadrupole mass spectrometer
• Agilent J&W DB-WAX Ultra Inert polar column (20 m × 0.18 mm, 0.18 µm)
• Agilent J&W DB-5ms Ultra Inert apolar column (20 m × 0.18 mm, 0.18 µm)
• Split/splitless inlets and autosampler (front and back)
• Inert compact splitter with deactivated fused silica tubing and flexible ferrules

Key results and discussion

Baseline separation of all 57 target compounds was achieved on both columns. Calibration curves over 1–100 mg/kg exhibited quadratic fits (ignoring the origin) with 1/x weighting and correlation coefficients above 0.997. Method transfer from GC/MSD to GC/TQ was seamless, preserving existing chromatographic and source parameters while obtaining optimal MRM transitions through automated optimization. Enhanced selectivity in MRM mode significantly reduced interferences and improved confidence in allergen quantitation.

Benefits and practical applications of the method

• High selectivity and reduced coelution improve accuracy and lower uncertainty.
• Automated MRM optimization accelerates method development and transfer.
• Dual-column approach provides confirmation of analyte identity in complex matrices.
• Applicable to regulatory compliance testing and quality control in cosmetic production.

Future trends and opportunities

As regulatory agencies continue to expand allergen lists, analytical methods will evolve to include higher-resolution mass spectrometry, enhanced data processing with artificial intelligence, and miniaturized or on-site testing solutions. Integration of automated workflows and real-time monitoring could further streamline compliance and safety evaluation.

Conclusion

The dual-column GC/TQ method on Agilent 8890 and 7000E instruments offers a rapid, selective, and reliable approach for quantifying 57 fragrance allergens and isomers in cosmetic products. Seamless transfer from GC/MSD methods and automated MRM optimization enhance productivity and data confidence, supporting regulatory compliance and consumer safety.

References

1. Regulation (EC) No 1223/2009 of the European Parliament and of the Council of 30 November 2009 on Cosmetic Products. Official Journal of the European Union, 2009.
2. Modernization of Cosmetics Regulation Act of 2022 (MoCRA). U.S. Food and Drug Administration, 2023.
3. Analytical Method to Quantify 57 Suspected Allergens and Isomers in Ready-to-Inject Fragrance Materials by Gas Chromatography and Mass Spectrometry. International Fragrance Association Analytical Working Group, 2016.