Analysis of Pharmaceuticals and Personal Care Products (PPCPs) as Contaminants in Drinking Water by LC/MS/MS Using Agilent Bond Elut PPL

Significance of the topic

Pharmaceuticals and personal care products (PPCPs) have emerged as ubiquitous trace contaminants in drinking water, raising concerns about potential human health effects and ecosystem disruption. Sensitive and robust analytical methods are essential to monitor and control these micropollutants at sub-ng/L levels, support regulatory compliance, and guide water treatment strategies.

Objectives and overview of the study

The study aimed to establish a rapid, reliable workflow for multiclass PPCP quantitation in drinking water by combining offline solid phase extraction (SPE) with high-performance LC/MS/MS. Four SPE sorbents were initially screened, and Agilent Bond Elut PPL was selected for its superior recovery across diverse analytes. Subsequent method optimization addressed sample loading conditions, elution steps, and analyte stability.

Methodology and used instrumentation

Sample preparation involved spiking 1 L municipal tap water with ascorbic acid (to quench residual chlorine), monopotassium phosphate, and EDTA, followed by internal standard addition. SPE cleanup used a 6 mL, 500 mg Bond Elut PPL cartridge with neutral sample loading, water wash, and two sequential elutions (acidic MeOH/ACN and basic MeOH/ACN). Eluates were combined, dried under nitrogen at 35 °C, and reconstituted in 10/90 MeOH/H2O.

Chromatography employed an Agilent 1290 Infinity II system with a ZORBAX RRHD Eclipse Plus C18 column (2.1×100 mm, 1.8 µm) at 40 °C, using a gradient of water and methanol (both containing ammonium formate, ammonium fluoride, and formic acid). Detection was performed on an Agilent 6470A triple quadrupole LC/MS with Jet Stream ESI in positive mode, using dynamic MRM transitions and MassHunter software for data acquisition.

Main results and discussion

Method validation demonstrated excellent linearity (R2>0.992) over 0.5–1,000 ng/L for 39 PPCPs. Method detection limits ranged from 0.5 to 13 ng/L, with average recoveries of 79–127% and RSDs below 20% at low (5 ng/L) and high (20 ng/L) spiking levels. Neutral loading preserved labile macrolides and β-lactams, while sequential acidic-basic elution maximized analyte recovery. Stability tests confirmed negligible degradation over 12 h under neutral conditions.

Benefits and practical applications

• The SPE-LC/MS/MS workflow offers high throughput and reproducibility for routine monitoring of PPCPs in drinking water.
• Low limits of quantification enable compliance with stringent regulatory guidelines and risk assessments.
• The method framework can be extended to environmental surface water and wastewater matrices.

Future trends and potential applications

Advances may include automated SPE platforms, further miniaturization for reduced solvent use, integration of high-resolution mass spectrometry for non-target screening, and expansion to emerging contaminants such as transformation products. Data analytics and machine learning could enhance method development and source apportionment.

Conclusion

An Agilent Bond Elut PPL SPE combined with LC/MS/MS provides a robust, sensitive, and reproducible method for multiclass PPCP analysis in drinking water. The validated workflow meets performance criteria for recovery, precision, and detection limits, and supports routine monitoring and environmental assessments.

References

• Method 1694 Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS, US EPA.
• Agilent Technologies Agilent Bond Elut PPL user guide, publication 5994-4162EN, 2021.
• Ye Z, Weinberg HS, Meyer MT. Trace Analysis of Trimethoprim and Sulfonamide, Macrolide, Quinolone, and Tetracycline Antibiotics in Chlorinated Drinking Water Using LC-ESI-MS/MS. Anal Chem. 2007;79:1135–1144.
• Gros M, Rodríguez-Mozaz S, Barceló D. Rapid Analysis of Multiclass Antibiotic Residues and Metabolites in Wastewater and River Water by UHPLC-QqLIT-MS/MS. J Chromatogr A. 2013;1292:173–188.
• 40 CFR Part 136 Appendix B Guidelines Establishing Test Procedures for the Analysis of Pollutants.
• Chinese regulation HJ 168-2020 Specification for Water Quality-Determination of PPCPs by LC/MS/MS.