Multi-component quantitative analysis of pharmaceuticals and personal care products in the environment by LC-MS/MS with fast polarity switching

Significance of the topic

Pharmaceuticals and personal care products (PPCPs) represent an emerging class of contaminants that persist in aquatic environments and pose ecological and human health risks due to their biological activity and endocrine-disrupting potential.

Objectives and study overview

This study aimed to develop a rapid, sensitive, and comprehensive multi-residue UHPLC-ESI-QqQ method with fast polarity switching for the simultaneous quantification of diverse PPCP compounds in environmental water samples. Performance was evaluated against dedicated single-polarity analyses.

Methodology

• Water samples from river and lake sites in Shiga, Japan were collected and spiked with 15 target PPCPs at concentrations ranging from 1 to 10000 ng/L.
• An optimized UHPLC gradient was applied to minimize matrix interference by retaining analytes at the column head and eluting unwanted components prior to target separation.
• Quantification was performed using selected reaction monitoring (SRM) with fast polarity switching to capture both positive and negative ions in a single run.

Used Instrumentation

• UHPLC System: Nexera with Shim-pack XR-ODSIII column (2.0 mm×50 mm, 1.6 μm); mobile phases: 0.1% formic acid in water (A) and acetonitrile (B); gradient from 0 to 100% B over 21 minutes; flow rate 0.4 mL/min; column temperature 40°C; injection volume 40 μL.
• MS System: LCMS-8080 triple quadrupole with ESI source; fast polarity switching (20 ms); nebulizing gas 3.00 L/min; curtain gas 3.50 L/min; drying gas 12.00 L/min; probe temperature 450°C; HSID temperature 300°C.

Main results and discussion

• The optimized gradient reduced matrix effects, achieving recoveries of 70–120% for most compounds.
• Limits of quantification ranged from 1 to 50 ng/L, with calibration linearity exceeding R² > 0.999 for all analytes.
• Fast polarity switching provided data quality comparable to separate positive and negative runs, simplifying workflow without sacrificing sensitivity.
• Long-term stability tests (100 injections over 10 hours) showed relative standard deviations below 4% for representative analytes.

Benefits and practical applications

• Enables simultaneous multi-class PPCP analysis in a single acquisition, improving throughput and efficiency.
• High sensitivity and robust quantification support environmental monitoring, regulatory compliance, and water quality assessment.
• Reduced solvent use and runtime compared to separate polarity methods lowers operational costs and resource consumption.

Future trends and potential applications

• Extension of the method to broader compound libraries, including transformation products and emerging contaminants.
• Application to diverse matrices such as wastewater, groundwater, and biosolids for comprehensive environmental surveillance.
• Integration with high-resolution MS and automation platforms for large-scale screening and data analytics.

Conclusion

The presented UHPLC-ESI-QqQ approach with fast polarity switching delivers a rapid, sensitive, and reliable multi-residue analysis of PPCPs in environmental waters, matching single-polarity performance while streamlining routine workflows for research and monitoring purposes.