Multi-Residue Analysis of Pharmaceuticals and Personal Care Products (PPCPs) in Water Using the ACQUITY UPLC H-Class System and the Xevo TQD Tandem Mass Spectrometer

Importance of the Topic

PPCPs are emerging contaminants detected at sub-ppt levels in water bodies worldwide. Their potential ecological and health impacts drive the need for sensitive and reliable analytical methods to monitor trace concentrations and diverse chemical structures.

Objectives and Overview

This work presents a single-injection UPLC-MS/MS method for simultaneous extraction, separation, and quantification of 78 acidic, basic, and neutral PPCPs in well and surface water. The approach emphasizes trace-level detection and broad chemical coverage.

Methodology and Instrumentation

Sample preparation relied on a tandem SPE stack combining Oasis MAX and MCX cartridges for reversed-phase, anion, and cation exchange, processing 1 L water at 10 mL/min. Eluates were collected in three fractions, evaporated, and reconstituted for analysis.

Chromatography was performed on an ACQUITY UPLC H-Class System with an HSS T3 2.1 × 100 mm, 1.7 μm column (60 °C, 0.45 mL/min), using a 10 mM ammonium formate pH 3.2 gradient in water/methanol.

Detection employed a Xevo TQD tandem mass spectrometer with ESI+/- mode, optimized capillary and cone voltages, MRM transitions for quantification and confirmation, and 82 compound parameters entered into a Quanpedia database.

Main Results and Discussion

Seventy-eight PPCPs were extracted effectively; five showed poor recovery in environmental matrices. Limits of detection reached sub-ppt levels. Reagent water blanks revealed four background analytes at 0.1–1 ppt. Calibration linearity (R2 0.991–0.997) was achieved for 58 compounds using three deuterated internal standards. Recoveries at 1 ppt ranged broadly across matrices. Matrix effects were <20% in reagent water, 20–50% in well water, and >50% for one-third of compounds in surface water.

Incurred residues included sulfamethoxazole at 0.97 ppt and atenolol at 0.32 ppt in well water, and multiple PPCPs <0.1 ppt in surface water.

Benefits and Practical Applications

• Sensitive multi-residue detection in a single injection
• Trace-level quantification across diverse PPCP classes
• Adaptable to environmental monitoring and regulatory compliance

Future Trends and Potential Applications

Method refinement may include enhanced SPE wash protocols, expansion of isotopic standards, integration of high-resolution MS, and automation of sample processing and data analysis. The approach can be extended to emerging contaminants and on-site screening.

Conclusion

The developed UPLC-MS/MS workflow offers robust, sub-ppt quantification of a wide range of PPCPs in water. Its combination of dual SPE and MRM profiling supports environmental surveillance and research. Further optimization will improve matrix tolerance and extend compound coverage.

References

1. http://www.epa.gov/ppcp/www.epa.gov/ppcp
2. A L Batt, M S Kostich, J M Lazorchak. Anal Chem. 2008, 80, 5021–5030.
3. B J Vanderford, S S Snyder. Environ Sci Technol. 2006, 40, 7312–7320.
4. S Reverte, F Borrull, E Pocurull, R M Marce. J Chromatogr A. 2003, 1010, 225–232.
5. J D Chahill, E Furlong, M R Burkhardt, D Kolpin, L G Anderson. J Chromatogr A. 2004, 1041, 171–180.
6. B Kasprzyk-Horden, D R Baker. J Chromatogr A. 2011, 1218, 1620–1631.
7. B Shao, D Chen, J Zhang, Y Wu, C Sun. J Chromatogr A. 2009, 1216, 8312–8318.