Analysis of Endocrine disrupting chemicals

Importance of the Topic

Endocrine disrupting chemicals (EDCs) such as androgens and estrogens are widely recognized for their ability to interfere with hormonal balance in humans and wildlife. Reliable analytical methods are essential for monitoring these compounds at trace levels in environmental and biological matrices to assess exposure risks and enforce regulatory standards.

Study Objectives and Overview

This application note describes the development and demonstration of a gas chromatography–mass spectrometry (GC-MS) method for the simultaneous analysis of seven steroidal endocrine disruptors: androsterone, dehydroepiandrosterone (DHEA), 17-α-estradiol, estrone, 17-β-estradiol, testosterone, and a derivatization by-product. Each analyte was prepared at 100 µg/mL to evaluate chromatographic separation, detection performance, and reproducibility.

Methodology and Instrumentation

Sample analysis was carried out on a Shimadzu GC-MS system equipped with an SH-I-1MS capillary column (30 m × 0.25 mm I.D., 0.25 µm film thickness). Key operational parameters included:

• Column temperature program: 100 °C initial, ramped at 10 °C/min to 320 °C, held for 10 min
• Injection: 1 µL splitless (0.5 min purge delay) using a single gooseneck inlet liner at 250 °C
• Carrier gas: helium at 1 mL/min (constant flow)
• Mass spectrometer: electron ionization (EI), scan range 40–700 amu, transfer line at 280 °C

Results and Discussion

The method achieved clear baseline separation of all target steroids within a single 30-minute run. Reproducible retention times and consistent mass spectral profiles enabled unambiguous identification. The absence of significant coeluting interferences demonstrates the suitability of the SH-I-1MS column for steroid analysis. Although quantitative figures are not provided here, the method’s sensitivity and selectivity support trace-level detection.

Benefits and Practical Applications

This GC-MS approach offers:

• High chromatographic resolution for structurally similar steroids
• Robust EI mass spectra for definitive compound confirmation
• Minimal sample preparation when paired with appropriate derivatization
• Applicability to environmental monitoring, clinical research, and regulatory compliance

Future Trends and Opportunities

Advancements poised to enhance steroid analysis include the integration of high-resolution mass spectrometry for improved detection limits, automated sample preparation workflows to increase throughput, and two-dimensional GC techniques for even greater separation power. Emerging methods such as microextraction and on-column derivatization may further streamline analysis.

Conclusion

The validated GC-MS protocol utilizing the SH-I-1MS column provides a reliable, high-throughput solution for the analysis of key endocrine disrupting steroids. Its balance of sensitivity, selectivity, and reproducibility makes it well suited for diverse analytical applications in research and quality control.

References

1. Shimadzu Corporation, Application Note ERAS-1000-0486, First Edition, September 2023.