Determination of Critical Elements in Foods in Accordance with US FDA EAM 4.7 ICP-MS Method

Significance of the Topic

Consumers require safe foods free of toxic elements; heavy metals and trace contaminants pose health risks; regulatory bodies like the US FDA set legal limits and standardized methods. Extending routine ICP-MS analysis enhances food safety programs and compliance.

Objectives and Study Overview

The study applied US FDA EAM 4.7 methodology using an Agilent 7800 ICP-MS with IntelliQuant data analysis to determine 20 elements in diverse food matrices. Goals included validating detection limits, QC procedures, and demonstrating rapid semiquantitative screening of unexpected contaminants.

Methodology and Instrumentation

Food samples and three SRMs were digested via microwave-assisted acid decomposition following EAM 4.7, using HNO3, HCl, and H2O2 in a closed-vessel MARS 6 system. An Agilent 7800 ICP-MS equipped with an ORS 4 helium collision cell (He-KED mode) measured all analytes, with enhanced He mode for selenium. High Matrix Introduction aerosol dilution handled up to 3 % TDS. Calibration standards in mixed acids covered 0.01 to 250 ppb. Internal standards compensated for drift. An SPS 4 autosampler ensured reproducible sample delivery. IntelliQuant Quick Scan acquired full mass spectra in He mode for up to 78 elements and calculated total matrix solids to monitor matrix effects.

Main Results and Discussion

Instrument detection limits were below EAM nominal criteria for all elements. SRM recoveries ranged 96 to 107 % meeting 80–120 % QC criteria. Fortified method blanks and spiked samples achieved recoveries within ±20 %. Continued calibration verification over 12 hours showed stable ISTD recoveries within ±10 %. Quantitative analysis of six real foods revealed expected element profiles; dark chocolate contained higher Cd and Pb yet remained below EU and FDA maximum levels. IntelliQuant identified titanium in powdered donuts and tungsten and nickel in dark chocolate, confirmed by isotope template fits.

Benefits and Practical Applications

• Preset methods and autotune accelerate setup.
• Single-gas He cell operation removes interferences without new overlaps.
• Wide dynamic range measures major and trace elements in one run.
• IntelliQuant enables rapid suspect screening, confirms unexpected analytes, and tracks matrix load to optimize maintenance.

Future Trends and Applications

Integration of semiquantitative full-spectrum screening into routine workflows for rapid compliance checks Emerging collision cell gases and advanced algorithms will further reduce interferences and improve sensitivity Miniaturized high-throughput digestion platforms will shorten prep times in regulatory and QA/QC labs Expanded spectral template libraries will enhance detection of novel food contaminants

Conclusion

The Agilent 7800 ICP-MS combined with FDA EAM 4.7 digestion and IntelliQuant provides robust, accurate multi-element food analysis in a single run. The approach meets regulatory QC criteria, offers long-term stability, and delivers rapid semiquantitative screening to support food safety monitoring.

References

1 US FDA Elemental Analysis Manual EAM 4.7 February 2020
2 Agilent Enhanced Helium Mode for ICP-MS publication
3 Agilent High Matrix Introduction technology brief
4 Proper W et al Agilent 7900 with UHMI for high salt matrices
5 Agilent ICP-MS MassHunter IntelliQuant brochure
6 Nelson J et al Spectroscopy online 2021
7 Cunningham WC et al US FDA EAM Terminology 2014
8 Nieburg O Chocolate cadmium and lead risk 2016
9 EU regulations on cadmium in food
10 US FDA guidance on lead in candy