Agilent ICP-MS Journal (August 2011 – Issue 47)

Importance of the Topic

ICP-MS combined with separation and reaction cell techniques has become indispensable for trace and speciation analysis in nutrition, pharmaceuticals and environmental monitoring. Detailed selenium speciation supports product efficacy and regulatory compliance. Modern elemental impurity methods aligned with USP<232>/<233> ensure patient safety by accurately quantifying toxic metals. Rapid 129I screening by ICP-MS enhances environmental assessments. Robust manufacturing and global training initiatives maintain high instrument availability and analytical expertise.

Objectives and Overview of the Studies

• Develop and validate LC-ICP-MS methods with mass balance calculations for selenium speciation in Se-enriched yeasts.
• Demonstrate ICP-MS analysis of 16 elemental impurities in pharmaceutical ingredients according to revised USP<232>/<233> protocols.
• Establish O₂ reaction mode ICP-MS for fast, low-ppt monitoring of radioactive iodine-129 in environmental and food samples.
• Review ICP-MS production recovery following the 2011 Japanese earthquake and document customer training events.

Methodology and Instrumentation

• Selenium speciation: Agilent 7700x ICP-MS coupled to Agilent 1260 LC with Zorbax C8 column; enzymatic extraction in Tris buffer; microwave acid digestion; MassHunter software with compound independent calibration (CIC).
• Pharmaceutical impurity analysis: Agilent 7700x ICP-MS in helium KED mode (ORS3), HCl/HNO₃ digestion, High Matrix Introduction (HMI) for robustness; validation at 0.5J–1.5J spike levels per USP<233>.
• 129I monitoring: Agilent 7700x ICP-MS using O₂ reaction mode to remove 129Xe overlaps; calibration with NIST 3231 standards; sub-2 ppt detection limits.
• Manufacturing and training: ICP-MS production at Hachioji facility supported by resilient supply chain; Agilent Academy ICP-MS training at Bangalore Center of Excellence.

Main Results and Discussion

• Selenium speciation: 70–90% of total Se extracted into soluble fraction; selenomethionine comprises ~66% of soluble Se; recoveries 89–97%; mass balance >96% using CIC allowed quantification of unknown species.
• Pharma impurity method: Recoveries of 25 elements ranged 86–118%; precision <20% RSD; secondary isotopes confirmed analyte identity; method meets USP criteria for accuracy, precision and specificity.
• 129I analysis: O₂ reaction mode eliminated 129Xe interference; linear calibration at low ppt; background equivalent concentration and detection limit ~1 ppt; precision <10% RSD; analysis in minutes with minimal sample prep.
• Manufacturing recovery: Full production capacity restored within two months; no shipment delays; R&D timelines largely unaffected; active support for disaster-affected regions.

Benefits and Practical Applications of the Methods

• Enables comprehensive speciation profiles for quality control of nutritional supplements.
• Offers reliable, high-throughput screening of elemental impurities in APIs and excipients under current regulatory frameworks.
• Delivers rapid screening of radioactive iodine for environmental and food safety monitoring without complex radiochemistry.
• Ensures global instrument availability and user proficiency through robust supply chains and dedicated training programs.

Future Trends and Potential Applications

Integration of ICP-MS with advanced separation techniques and reaction gases will expand capabilities for isotope‐specific analyses. Performance‐based regulations will drive wider adoption of multi‐element speciation and isotope ratio measurements in pharmaceuticals, food safety and environmental science. Automation, remote operation and AI‐enhanced data processing are expected to improve throughput, reproducibility and data interpretation.

Conclusion

The Agilent 7700 Series ICP-MS, when coupled with LC and reaction cell technologies, provides sensitive, robust and versatile solutions for trace and speciation analysis across diverse applications. Validated methods for selenium speciation, pharmaceutical impurity quantification and 129I monitoring meet stringent regulatory requirements. Resilient manufacturing processes and global training initiatives ensure sustained support for critical analytical workflows.

References

• Jacques KA. Feed Compounder 2002, 14–21.
• Goenaga-Infante H et al. Journal of Analytical Atomic Spectrometry 2005, 20, 864–870.