Advancing Endocrine Disrupting Compound Analysis Through Integrated Technology and Workflow Solutions

Significance of the Topic

Endocrine Disrupting Compounds (EDCs), including natural and synthetic estrogens and alkylphenol derivatives, can affect hormonal balance in humans and wildlife at part-per-trillion levels. Reliable monitoring of these contaminants in groundwater, surface water, and sewage effluent is essential for public health protection, environmental stewardship, and regulatory compliance.

Study Objectives and Overview

This study demonstrates an end-to-end workflow combining solid-phase extraction, ultra-performance liquid chromatography, and tandem mass spectrometry to achieve rapid, sensitive quantification of multiple EDCs. Key aims:

• Enrichment of EDCs from diverse water matrices using Oasis HLB SPE.
• Simultaneous targeted MRM and full-scan data acquisition via RADAR™ on Xevo TQ MS.
• Automated method development using IntelliStart™ software.

Methodology

Samples (groundwater, river water, sewage effluent) were spiked and processed through Oasis HLB cartridges following established environmental protocols. Chromatographic separation utilized an ACQUITY UPLC BEH C18 column (2.1×50 mm, 1.7 µm) with a gradient from 0.05% NH4OH (aqueous) to methanol over a 5.3 min runtime. Mass spectrometry employed negative-mode ESI on a Xevo TQ MS in RADAR Dual Scan-MRM mode, capturing both MRM transitions and full-scan spectra. IntelliStart automated optimization of precursor/product ions, cone voltage, and collision energy. TargetLynx processed quantitative data, while TrendPlot tracked internal standard consistency across batches.

Instrumentation

• ACQUITY UPLC System with BEH C18 column.
• Xevo TQ MS equipped with RADAR™ and ScanWave™ technologies.
• Waters Oasis HLB SPE cartridges (5 cc/200 mg).
• IntelliStart™, MassLynx®, TargetLynx™, and TrendPlot software.

Key Results and Discussion

EDCs were reproducibly detected at sub-ng/L levels following SPE enrichment. Chromatography achieved baseline separation of 17α- and 17β-estradiol in under 3.2 min, enabling high throughput. Groundwater, river water, and sewage extracts spiked at 5 ng/L equivalent produced clean MRM peaks. TrendPlot identified outlier injections via internal standard monitoring, enhancing QC. RADAR full-scan acquisition revealed co-eluting humic/fulvic substances and linear alkylbenzene sulfonates, guiding method refinement. Retrospective analysis identified pentachlorophenol at 20 ng/L from full-scan data, demonstrating discovery capabilities.

Benefits and Practical Applications

• Accelerated method development reduces resource demands.
• High sensitivity/selectivity supports regulatory monitoring of water quality.
• Concurrent qualitative and quantitative data improves sample characterization.
• Automated tracking of performance and matrix effects ensures data reliability.

Future Trends and Opportunities

Advancements may include high-resolution non-target screening, machine learning for spectral interpretation, miniaturized field units for real-time EDC surveillance, and expanded open-access data repositories for retrospective analysis and contaminant discovery.

Conclusion

The integrated SPE-UPLC-TQ MS workflow with IntelliStart and RADAR functionality offers a robust, high-throughput solution for trace-level EDC analysis in complex environmental waters, facilitating informed decision-making and regulatory compliance.

References

1. Colborn T, Soto AM, vom Saal FS. Environmental Health Perspectives. 1993;101(5):378–384.
2. Pillon AP, et al. Environmental Health Perspectives. 2005;113(3):278–284.
3. Díaz-Cruz MS, et al. Journal of Mass Spectrometry. 2003;38(9):917–923.