Multi-Residue Analysis of Pharmaceuticals, Personal Care Products (PPCPs) and Pesticides in Water by Direct Injection Using LC-MS/MS

Significance of the Topic

Water contamination by trace-level pharmaceuticals, personal care products and pesticides has become a global concern due to potential risks to human health and the environment. Regulatory authorities in the European Union continue to expand watch lists and tighten limits under the Water Framework Directive and Drinking Water Directive. Fast, sensitive, and environmentally friendly methods are needed to screen a growing number of diverse analytes in different water matrices without extensive sample cleanup.

Study Objectives and Overview

This study presents a multi-residue method for the direct injection analysis of over 190 pharmaceuticals, personal care products (PPCPs) and pesticides, including degradation products, in tap water, bottled mineral water and surface water. The goal was to demonstrate compliance with emerging EU monitoring requirements, evaluate method performance at trace levels (10–125 ng/L), and assess productivity gains from minimal sample preparation.

Methodology and Instrumentation

Samples were acidified to 0.01% acetic acid, aliquoted into certified glass vials and analyzed by UPLC–MS/MS without solid-phase extraction or concentration steps. Matrix-matched calibration was performed in bottled mineral water over nine levels (5–1000 ng/L). Spiked recovery experiments at 10, 25 and 125 ng/L with six replicates each assessed trueness and precision. Chromatographic separation used an ACQUITY Premier HSS T3 column (2.1 × 100 mm, 1.8 µm) at 45 °C with a gradient of 0.01% acetic acid in water and 0.01% acetic acid in 50:50 methanol:acetonitrile. MS detection employed fast polarity switching in both positive and negative ESI modes.

Instrumentation Used

• ACQUITY Premier FTN UPLC system
• Xevo TQ Absolute tandem quadrupole mass spectrometer
• ACQUITY Premier HSS T3 Column, 1.8 µm, 2.1 × 100 mm

Main Results and Discussion

Calibration was linear (98% of compounds with R² > 0.99 using 1/X weighting) across 5–1000 ng/L. Retention times were stable (<3.2% RSD) and peak shapes Gaussian in all matrices. In the most challenging surface water, average trueness was 92% (range 57–131%) with RSD of 5% and 99% of results below 20% RSD. Over 150 analytes achieved limits of quantification of 10 ng/L, and signal-to-noise ratios above 100 at 10 ng/L were observed for key targets such as metconazole.

Benefits and Practical Applications

• High sensitivity for trace-level detection without lengthy sample preparation
• Increased throughput and faster turnaround in routine monitoring laboratories
• Alignment with green analytical chemistry by minimizing solvent use and waste
• Suitability for EU compliance screening of multi-class analytes in diverse water types

Future Trends and Potential Applications

Further method refinement could include isotopically labeled internal standards to correct for minor matrix effects and losses. Expanding the analyte panel to new emerging contaminants and incorporating high-resolution mass spectrometry may enhance selectivity. Automation of data processing and integration with online monitoring platforms could support real-time water quality surveillance.

Conclusion

The direct injection LC–MS/MS method on the ACQUITY Premier System coupled with the Xevo TQ Absolute provides a robust, sensitive and high-throughput solution for multi-residue analysis of PPCPs and pesticides in drinking and surface waters. The workflow meets stringent EU regulatory requirements, delivers excellent accuracy and precision at trace levels, and supports greener laboratory practices.

Reference

1. US EPA. Contaminants of Emerging Concern Including Pharmaceuticals and Personal Care Products, 2025.
2. Directive (EU) 2020/2184 on the Quality of Water Intended for Human Consumption, 2020.
3. Directive 2000/60/EC Establishing a Framework for Community Action in the Field of Water Policy, 2000.
4. Commission Implementing Decision (EU) 2022/1307 Establishing a Watch List of Substances for Water Monitoring, 2022.
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11. ISO 21253–2:2019 Water Quality — Multi-compound Class Methods Part 2, 2019.