LC/MS, LC/MS/MS, LC/QQQ
IndustriesFood & Agriculture
ManufacturerShimadzu
Significance of the topic
Perfluoroalkyl and polyfluoroalkyl substances are persistent environmental pollutants that bioaccumulate in food chains. Their presence in fish and pet food poses health risks, making reliable analytical methods essential for regulatory compliance and consumer safety.
Study objectives and overview
This work describes a single-laboratory validation of a rapid QuEChERS extraction coupled with LC-MS/MS for quantifying 30 PFAS in fish and pet food. The aim was to meet AOAC SMPR 2023.003 criteria, including stringent requirements for EU regulated compounds.
Methodology and instrumentation
- Sample preparation using QuEChERS with weak anion exchange SPE cleanup
- Fish tissue: 10 g sample, spiked, extracted with acetonitrile
- Pet food: 2 g sample, spiked, extracted with water and acetonitrile
- Isotope dilution quantification with matrix-matched standards
- Analysis on Shimadzu Nexera liquid chromatograph coupled to LCMS-8060NX triple quadrupole
- Nine-minute gradient for separation, optimized for peak shape and S/N
Key results and discussion
Calibration exhibited linearity across required ranges. Limits of quantification for all PFAS met or exceeded SMPR thresholds without sample preconcentration. Recoveries ranged from 92 to 119 and repeatability RSD values were below 15 for all analytes. Baseline resolution was achieved for regulatory PFAS isomers and separation from matrix interferences such as bile acids.
Benefits and practical applications
- High throughput analysis with only nine minutes per run
- Simultaneous quantification of 30 PFAS in complex food matrices
- Compliance with global regulatory standards for fish and pet food
Future trends and potential uses
Advancements may include expanding the scope to emerging PFAS, improving sensitivity further with new ionization techniques, and applying this workflow to other food and environmental matrices for comprehensive monitoring.
Conclusion
The validated QuEChERS-LC-MS/MS method on the Shimadzu LCMS-8060NX platform delivers robust, rapid, and regulatory-compliant quantification of 30 PFAS in fish and pet food, supporting food safety and quality control efforts.
Reference
- AOAC SMPR 2023.003 Determination of PFAS in food matrices
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