LC/MS, LC/MS/MS, LC/QQQ
IndustriesEnvironmental
ManufacturerShimadzu
Importance of the Topic
Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants with potential health risks, used widely in industrial and consumer products. Although PFAS in drinking water have been extensively studied, the prevalence of these compounds in bottled water containers remains less characterized. Understanding PFAS content in commercial bottled water is essential for assessing consumer exposure and guiding regulatory standards.
Aims and Study Overview
This study aimed to develop a rapid, direct-injection LC-MS/MS method for quantifying 24 target PFAS and 19 isotopically labeled surrogates in bottled water and to evaluate the influence of bottle material and water source on PFAS levels.
Methodology and Instrumentation
Sample Preparation:
- Bottled water samples (spring and purified) were diluted 1:1 with methanol containing 0.1% acetic acid and spiked with isotopic surrogates.
- Samples were vortexed, filtered through 0.2 μm syringe filters, and directly injected.
Chromatography and Mass Spectrometry Conditions:
- Column: Restek Raptor C18 (2.1×150 mm, 2.7 μm); PFAS delay column to prevent system carryover.
- Mobile phases: A (20 mM ammonium acetate in 5% acetonitrile), B (10 mM ammonium acetate in 95% acetonitrile), gradient 0–21 min.
- Autosampler: Shimadzu Nexera X2 SIL-30AC; MS: Shimadzu LCMS-8050 triple quadrupole; injection volume 30 μL.
- MRM transitions optimized for each analyte; run time 21 min.
Used Instrumentation
- Shimadzu Nexera X2 SIL-30AC autosampler
- Shimadzu LCMS-8050 triple quadrupole mass spectrometer
- Restek Raptor C18 analytical column; PFAS delay column
- Syringe filters (0.2 μm) and high-purity solvents with PFAS-free handling
Main Results and Discussion
Method performance:
- LOQ established at 10 ppt.
- Recoveries for an 80 ppt standard ranged from 87.6% to 129.5%, with relative standard deviations below 10% for most compounds.
Sample analysis:
- Only two PFAS—perfluorobutanoic acid (PFBA) and 6:2 fluorotelomer sulfonate (6-2 FTS)—were detected above LOQ.
- Plastic bottles showed measurable PFAS; recycled plastic contained the highest total PFAS levels.
- Glass and cardboard containers had no detectable PFAS.
- PFBA concentration was highest in a spring water sample stored in a specific plastic bottle.
These findings indicate that both the bottle material and water source contribute to PFAS levels in bottled water, though further investigation with larger sample sets is needed.
Benefits and Practical Applications
- Rapid, minimal-prep direct injection method suitable for high-throughput monitoring.
- Performance meets or exceeds FDA and EPA draft method requirements for PFAS in aqueous matrices.
- Applicable for quality control in bottled water production and compliance testing.
Future Trends and Potential Applications
Future work may include implementing isotopic dilution calibration for improved quantitation, extending the method to other food packaging materials and water sources, and integrating high-throughput screening protocols to support regulatory monitoring and risk assessment.
Conclusion
The developed LC-MS/MS direct injection method provides reliable, sensitive detection of PFAS in bottled water. Results highlight that plastic materials, especially recycled plastic, can introduce PFAS into water, while glass and cardboard appear PFAS-free under the tested conditions. This approach supports rapid screening and informs safer packaging choices and regulatory guidelines.
References
- FDA Makes Available Testing Method for PFAS in Foods and Final Results from Recent Surveys.
- FDA Makes Available Results from Second Round of Testing for PFAS in Foods from the General Food Supply.
- Environmental Science and Technology. Polyfluorinated Compounds: Past, Present, and Future. 2011.
- International Bottled Water Association. Recommended PFAS Levels in Bottled Water.
- US EPA. Basic Information about PFAS.
- Prakash B., Marfil-Vega R., Gilles C., Lipps W. Analysis of PFAS in Non-Drinking Water Matrices Using LC-Triple Quad Mass Spectrometer. Pittcon 2020 Poster.
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