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Excellent choices for food & agriculture applications

Guides | 2011 | Agilent TechnologiesInstrumentation
GC/MSD, Sample Preparation, GC/SQ, HPLC, ICP/MS, ICP-OES, AAS, Speciation analysis
Industries
Environmental, Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Significance of Topic


Ensuring the safety and quality of food and agricultural products requires sensitive, accurate methods to detect trace and toxic elements—such as lead, cadmium, mercury, arsenic, and selenium—and to characterize their chemical forms. Contamination by heavy metals poses health risks and impacts consumer confidence and regulatory compliance; speciation of elements like arsenobetaine and methylmercury is crucial for assessing toxicity.

Objectives and Study Overview


This collection of application studies demonstrates cutting-edge approaches for rapid, direct, and speciation-capable analysis of trace elements in diverse matrices—water, milk powder, fish and shellfish tissues, plant materials, and distilled spirits—using techniques including ICP-OES, ICP-MS (with collision/reaction cell), HPLC-ICP-MS, GC-MS, AAS with cold vapor and hydride generation, and vapor-generation AA. Emphasis is placed on minimizing sample preparation, avoiding hazardous reagents, and sustaining high throughput.

Methodology and Instrumentation


  • Direct ICP-OES for milk powder: Axi-viewed simultaneous plasma with internal standards (Sc, Cs) enabled robust major and trace element quantitation in 2% w/v suspensions, avoiding wet ashing and dilution.
  • ICP-MS with Octopole Reaction System: Helium collision mode removed Ar-, C- and Cl-based interferences in whisky and food digests, allowing rapid multi-element screening including low-ppt Hg.
  • HPLC-ICP-MS speciation: Isocratic separation of arsenobetaine and other As species in fish extracts with CCD detection; methanol-enhanced ionization and sample dilution circumvented matrix effects.
  • GC-MS isotope dilution: Electron-impact MS of methylmercury in tuna, using 201Hg-enriched spike and SPME extraction, delivered accurate speciation quantitation.
  • AAS with hydride and cold-vapor generation: VGA-76 accessory on AA-1475 enabled ppt-level detection of As, Sb and Se in acid-digested orchard leaves using non-perchloric mixtures.

Key Results and Discussion


Direct ICP-OES analyses matched certified values for milk-powder reference materials, confirming internal-standard correction of viscosity and ionization biases. Whisky screening by ICP-MS/ORS-He revealed category-specific element profiles and highlighted Pb leaching from crystal decanters. HPLC-ICP-MS achieved baseline AsB separation in under 10 min, with detection limits ~0.04 ng/g; interlaboratory feasibility studies confirmed its reliability. GC-MS isotope-dilution of methylmercury in tuna produced recoveries within 1% of certified values. Vapor-generation AAS on plant digests yielded arsenic and antimony results within uncertainty of NBS orchard-leaf guidelines.

Benefits and Practical Applications


  • Streamlined workflows eliminate lengthy chemical digestions—enabling direct or semi-direct analysis.
  • Collision/reaction cells in ICP-MS ensure robust interference removal under a single set of conditions.
  • Speciation capabilities provide toxicologically relevant data (AsB, MeHg, inorganic vs. organic As and Se).
  • High throughput—up to 50 sample runs per day—meets large-scale screening demands.
  • Compliance with regulatory limits for food safety and QC/QC laboratory accreditation.

Future Trends and Potential Uses


Advances in high-resolution and tandem mass spectrometry will further refine speciation and lower detection limits. Miniaturized and automated sample-prep platforms, such as on-line digestion and SPME robotics, promise greater throughput. Expansion into emerging contaminants—organometallic species and nanomaterials—will require hybrid platforms combining chromatographic separation with element-specific detection. Integration with data science and chemometric tools can enable real-time monitoring of food chains.

Conclusion


The suite of methods presented demonstrates that modern element-specific and speciation-capable instruments offer rapid, accurate, and high-throughput solutions for monitoring toxic and essential trace elements in complex food and agricultural matrices. Through strategic application of collision/reaction cells, internal standardization, isotope dilution, and enhanced sample-prep protocols, laboratories can achieve reliable compliance testing and research data with minimized hazards and processing times.

Used Instrumentation


  • Agilent 5100/5110/5800/5900 ICP-OES (axial/simultaneous).
  • Agilent 7500i/cx ICP-MS with Octopole Reaction System.
  • Agilent 1100 HPLC coupled to 7500i ICP-MS.
  • Agilent 6890N GC with 5973 MSD (for methylmercury SPME-GC-MS).
  • Agilent AA-1475 AA with VGA-76 hydride/cold-vapor accessory.
  • Microwave digestion systems (CEM Mars).

References


  • Gelman A., Varian AA-44, 1985.
  • Hoenig M., de Borger R., Spectrochim. Acta 38B 873, 1983.
  • Clinton O., Anal. Chem. 102 187, 1977.
  • McKiernan J.W. et al., Anal. At. Spectrom. 14 607, 1999.
  • Centineo G. & García Alonso J.I., Anal. At. Spectrom. 23 1106, 2008.

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