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Heavy Metal Index

Determination of soluble toxic arsenic species in alga samples by microwave-assisted extraction and high performance liquid chromatography-hydride generation-inductively coupled plasma-atomic emission spectrometry

Source

García Salgado et al. developed a microwave-assisted water extraction and HPLC-HG-ICP-AES method for soluble arsenic species in algae.

Page snapshot
Cited by7 pages
Metals measured2
Evidence tierB
Year2006

Overview

García Salgado et al. developed a microwave-assisted water extraction and HPLC-HG-ICP-AES method for soluble arsenic species in algae. The paper analyzes Sargassum CRM material, Chlorella vulgaris, market Hizikia fusiformis dry material, and market Laminaria digitata capsules. Total arsenic, inorganic arsenic species, and methylated arsenic species are kept separate below.

Key numbers

The paper reports total arsenic in the four algae/materials as µg g−1 arsenic, dry-weight context:

Sample/materialTotal arsenic
NIES No. 9 Sargassum CRM106 ± 6 µg g−1
Hizikia fusiformis88 ± 6 µg g−1
Laminaria digitata41 ± 4 µg g−1
Chlorella vulgaris39 ± 3 µg g−1

Table 3 compares extraction efficiencies for three consecutive 8 mL deionized-water extraction steps:

Sample/materialUltrasonic focused probe (20 kHz, 30 s)Microwave oven (90°C, 5 min)
NIES No. 9 Sargassum CRM65 ± 3%98 ± 5%
Hizikia fusiformis69 ± 4%88 ± 5%
Laminaria digitata67 ± 4%78 ± 4%
Chlorella vulgaris64 ± 3%85 ± 5%

Table 5 reports quantitative arsenic species in µg g−1 arsenic (mean ± standard deviation, n = 3) by HPLC-HG-ICP-AES:

Sample/materialAs(III)As(V)MMADMATotal As extractedSpeciation recovery
NIES No. 9 Sargassum CRMnot detected72 ± 3not detectednot detected113 ± 564 ± 3%
Hizikia fusiformisnot detected62 ± 2not detectednot detected77 ± 380 ± 3%
Chlorella vulgaris6.1 ± 0.411.8 ± 0.52.2 ± 0.315 ± 233 ± 5106 ± 9%

For Laminaria digitata, none of the four target species was identified by HPLC-HG-ICP-AES. The paper reports an unknown arsenic species in the HPLC-ICP-AES chromatogram, eluting in the dead volume and estimated as 7.0 ± 1.1 µg g−1 arsenic.

Table 4 reports detection limits as absolute ng As: As(III) 0.5, DMA 2.0, MMA 1.0, and As(V) 2.0. Relative standard deviations were As(III) 3.3%, DMA 4.5%, MMA 3.7%, and As(V) 4.8%.

Table 6 spiked Hizikia stability recoveries were As(III) 95 ± 3%, DMA 92 ± 8%, MMA 115 ± 9%, and As(V) 93 ± 7%; for As(V), the source subtracts the 16.8 µg already present in the sample from the found concentration.

Methods (brief)

Approximately 200 mg of algae was extracted with 8 mL deionized water by microwave heating at 90°C for 5 min; the extraction was repeated three times, then extracts were centrifuged and filtered. Total arsenic was measured by ICP-AES after microwave digestion. Arsenic species studied were As(III), As(V), MMA, and DMA, separated on an anion-exchange Hamilton PRP-X100 column and detected by HPLC-HG-ICP-AES. Hydride generation used 4 M HCl, 0.5% (w/v) NaBH4, and 350 kPa carrier argon pressure.

Implications

The market Hizikia result is the most directly relevant food occurrence row in this paper: total arsenic 88 ± 6 µg g−1 with measured As(V) 62 ± 2 µg g−1 in the water extract. The Chlorella result is relevant to algae-based supplement context because it reports both inorganic and methylated soluble arsenic species. The Sargassum CRM is QA/context rather than a consumer product row, and the Laminaria capsule result should be treated cautiously because the target toxic species were not detected while an unidentified arsenic species was observed.

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Verification notes

  • Identity checks before writing found no existing DOI, raw-handle, or cite-key page for 10.1016/j.chroma.2006.06.083, MFK_10-1016-j-chroma-2006-06-083, or garcia-salgado2006-soluble-arsenic-algae.
  • All Key numbers were rechecked against /tmp/hmi-seaweed-003.txt, extracted with pdftotext -layout, especially Tables 3, 4, 5, and 6 plus the total-arsenic values in the sample-description text.
  • Speciation check: Table 5 values are kept as As(III), As(V), MMA, and DMA. Total arsenic is not substituted for inorganic arsenic.
  • Units are preserved as µg g−1, %, ng As, and µg; no conversions were performed.
  • Evidence tier B reflects peer-reviewed method/speciation data with exact species and method validation, but a small sample set and inclusion of a CRM/research material rather than a full market survey.
  • Brand firewall: no sampled brands are reported; market purchase is retained only at category level.

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.

CommitDateChangeDescription
b01ec52c32026-08-04major1 section added
3171d069e2026-08-02major1 section added
90a2f9a382026-07-30major1 section added and 1 removed; narrative text revised
eaa8eeeed2026-07-27major1 section added
50de6ab212026-07-27minorNarrative text revised