Overview
This paper develops and validates an optimized HPLC-ICP-MS method for iAs determination in a range of food matrices including seaweed, rice, grass silage, and insect proteins, using a design of experiments (DoE) approach to optimize chromatographic conditions. The method is validated against certified reference material (hijiki certified reference material) achieving 99±9% recovery for iAs. The paper also reports iAs concentrations in the tested matrices, establishing that Laminaria digitata can have iAs comprising more than 50% of total arsenic in some samples, with regulatory implications under the EU maximum level for iAs in seaweed.
Key numbers
- Certified reference material recovery: 99±9% for iAs in hijiki seaweed (excellent method validation)
- Laminaria digitata iAs: up to >50% of total As in some samples; specific concentration values reported (see source tables)
- Fucus spp.: lower iAs/tAs ratio than Laminaria
- Saccharina latissima: iAs lower than Laminaria, consistent with brown macroalgae literature
- Asparagopsis taxiformis: contains organoarsenic brominated compounds that may interfere with standard iAs methods; this paper addresses that interference
- Porphyra spp. (nori): low iAs, predominantly arsenosugars
- Rice: method validated and suitable for iAs determination in rice; values consistent with published literature
- Insect proteins: novel application; iAs present at trace levels in insect-derived proteins tested
- Grass silage: included as an animal feed matrix; iAs measurable with the method
- EU regulatory context: EU Regulation 2023/915 sets maximum levels for iAs in specific seaweed species (e.g., Laminaria digitata, hijiki); this method is designed to support compliance testing
Methods (brief)
HPLC-ICP-MS with anion exchange column (Hamilton PRP-X100 or equivalent); mobile phase optimization by DoE (Box-Behnken design) varying pH, buffer concentration, and methanol percentage; LOD and LOQ for iAs determined; extraction by dilute HNO3 microwave-assisted digestion; certified reference material (NIES CRM No. 18 hijiki) used for method validation. Total As measured by ICP-MS without chromatography for comparison.
Implications
Certification: This is a directly applicable methods reference for iAs testing in seaweed and novel protein ingredients. The DoE-optimized method achieves excellent recovery and is validated against a certified reference. The EU regulatory context (Regulation 2023/915 iAs limits in seaweed) is explicitly addressed.
Courses: Exemplary paper for teaching HPLC-ICP-MS speciation methodology; also demonstrates DoE optimization approach for chromatographic method development.
App: Seaweed ingredients have complex arsenic speciation; iAs fraction can be >50% in Laminaria. Total As alone is insufficient for risk characterization in seaweed-derived ingredients.
Microbiome: Not applicable.
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Update history
The five most recent substantive edits to this page, classified major (evidence or structure moved), correction (a published value or statement was wrong and has been fixed), or minor (narrative rewritten without changing the underlying evidence). Each description is derived from what the edit did to this page; the linked commit is the authoritative record, routine regeneration passes are excluded, and the full version history lives in git. When DOI minting comes online (see schema docs), each entry below will also link to a version-pinned DataCite DOI.
| Commit | Date | Change | Description |
|---|---|---|---|
| a8052bb | 2026-08-09 | major | 6 sections added; narrative text revised |