PPCP Analysis in Bottled, Tap and Surface Water using Time De-Coupled Chromatography

Importance of the Topic

Contamination of drinking and surface waters by pharmaceuticals and personal care products (PPCPs) poses risks to ecosystems and human health. Trace-level monitoring of these micropollutants requires highly sensitive, rapid and robust analytical workflows to support environmental surveillance and regulatory compliance.

Study Objectives and Overview

This work evaluates Time De-Coupled Chromatography (2D mode) coupled with LC-MS/MS for quantifying a broad suite of PPCPs in bottled, tap and surface water. Key aims are to minimize sample preparation time, reduce required sample volume and achieve sub-ppt detection limits.

Methodology and Instrumentation

Sample Preparation and Chromatography

• Solid-phase extraction (SPE) using mixed sorbents (Oasis HLB, MAX, MCX) for simultaneous enrichment of acidic and basic PPCPs.
• Automated AT-column dilution for direct injection of aqueous or organic extracts (up to 1 mL) without evaporation/reconstitution.
• Time De-Coupled 2D chromatography enabling large-volume injections and fast transfer between trapping and analytical columns.

Instrumental Setup

• Waters ACQUITY UPLC system with two binary pumps, 1000 µL injection loop and trap column.
• BEH C18 and C8 columns for orthogonal separations.
• Triple quadrupole MS operated in multiple reaction monitoring (MRM) mode with electrospray ionization (ES+).

Main Results and Discussion

The method delivered detection limits down to 1 ppt for multiple PPCPs in 15 mL water samples. Spike recoveries at 10 ppt ranged from 70 % to 115 %, with linearity (r2) above 0.99. Analysis time per sample was reduced from over one hour to under 15 minutes. Direct injection of up to 1 mL extract provided 10× enrichment, eliminating lengthy evaporation steps. Precision and accuracy were maintained below 10 % RSD across water matrices.

Benefits and Practical Applications

• Trace-level detection (ppt) of diverse PPCPs.
• Minimal sample preparation (< 15 min) and reduced manual labor (~80 % time savings).
• Wide pH compatibility for acidic and basic analytes with mixed SPE sorbents.
• High throughput enabling environmental monitoring and QA/QC in water utilities and research laboratories.
• Robustness and reproducibility for routine analysis.

Future Trends and Applications

Further automation of SPE and on-line 2D coupling could enable field-deployable systems. Integration with high-resolution MS and data-driven quantification will broaden target lists. Green extraction solvents and miniaturized formats may reduce environmental footprint while extending the approach to other trace contaminants.

Conclusion

Time De-Coupled Chromatography combined with LC-MS/MS offers a rapid, sensitive and robust solution for ppt-level PPCP analysis in various water matrices. The streamlined workflow drastically cuts analysis time and sample volume, supporting high-throughput environmental monitoring and regulatory testing.

References

• Mallet CR. PPCP Analysis in Bottled, Tap and Surface Water using Time De-Coupled Chromatography. Waters Corporation; 2014.