Determination of 30 Per- and Polyfluoroalkyl Substances in Bovine Kidney

Importance of the Topic

Per and polyfluoroalkyl substances PFAS pose significant environmental and health challenges due to their persistence and potential toxicity. Monitoring PFAS levels in food products such as bovine kidney is essential to ensure food safety regulatory compliance and to protect public health. Development of robust analytical methods enables accurate quantitation of multiple PFAS in complex matrices and supports risk assessment and policy decisions.

Objectives and Study Overview

This study aimed to establish and validate a comprehensive workflow for determining 30 PFAS in bovine kidney tissue. The method integrates QuEChERS extraction with enhanced matrix removal EMR mixed-mode passthrough cleanup using the Agilent Captiva EMR PFAS Food II cartridge, followed by quantitation with an Agilent 6495D triple quadrupole LC MS system. Method performance was evaluated according to AOAC SMPR 2023.003 requirements including suitability sensitivity accuracy and precision.

Methodology and Instrumentation

Sample preparation involved homogenizing bovine kidney tissue spiking with isotopically labelled internal standards and performing QuEChERS extraction with acetonitrile containing 1% acetic acid and buffered salts. Enhanced matrix removal was achieved using Captiva EMR PFAS Food II cartridges followed by dilution and filtration. Chromatographic separation utilized an Agilent 1290 Infinity II UHPLC system equipped with ZORBAX RRHD Eclipse Plus C18 columns and a PFC delay column. Detection was performed on an Agilent 6495D triple quadrupole LC MS with Jet Stream iFunnel electrospray ionization controlled by MassHunter software.

Main Results and Discussion

Comparison with traditional dispersive SPE cleanup showed that EMR mixed-mode passthrough significantly improved PFAS recoveries across a range of analytes. Validated limits of quantitation were below or equal to regulatory thresholds for edible offal with core PFOS PFOA PFNA and PFHxS LOQs of 0.2 to 0.4 µg/kg. Method accuracy and precision met acceptance criteria with recoveries generally between 80 and 120% and relative standard deviations below 20% for core PFAS and within expanded criteria for other targets.

Benefits and Practical Applications

The proposed workflow offers a streamlined sample preparation that eliminates a drying step thereby reducing analysis time and complexity. High throughput capability and compliance with AOAC performance standards facilitate routine PFAS monitoring in food safety laboratories. The method can be readily adapted to other complex food matrices for regulatory surveillance and quality control.

Future Trends and Potential Applications

Advances may include automation of the EMR cleanup process integration with high resolution mass spectrometry for non targeted screening and expansion of target panels. Emerging regulatory requirements will drive demand for even lower detection limits and broader PFAS coverage. Coupling with novel ion mobility separation and data analysis tools could further enhance selectivity and throughput.

Conclusion

A rapid reliable and validated method for quantifying 30 PFAS in bovine kidney using QuEChERS extraction EMR mixed-mode cleanup and LC MS MS detection was developed. The approach meets AOAC SMPR 2023.003 performance criteria and supports accurate PFAS determination in complex food matrices.

References

1. AOAC International Standard Method Performance Requirements SMPR 2023.003 for Per and Polyfluoroalkyl Substances in Produce Beverages Dairy Products Eggs Seafood Meat Products and Feed 2023
2. Zhao L Giardina M Parry E Determination of 30 Per and Polyfluoroalkyl Substances in Infant Formula Milk and Eggs Using Agilent Captiva EMR PFAS Food II Pass Through Cleanup and LC MS MS Detection Agilent Technologies Application Note 5994-7366EN 2024