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SPE HG-AAS method for the determination of inorganic arsenic in rice—results from method validation studies and a survey on rice products

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Authors:
  • Rasmussen, Rie Romme ;
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    Orcid logo0000-0002-5889-8496
    National Food Institute, Technical University of Denmark
  • Qian, Yiting ;
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    National Food Institute, Technical University of Denmark
  • Sloth, Jens Jørgen
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    Orcid logo0000-0002-3636-8769
    National Food Institute, Technical University of Denmark
DOI:
10.1007/s00216-013-6936-8
Abstract:
The present paper describes the development, validation and application of a method for inorganic arsenic (iAs) determination in rice samples. The separation of iAs from organoarsenic compounds was done by off-line solid-phase extraction (SPE) followed by hydride generation atomic absorption spectrometry (HG-AAS) detection. This approach was earlier developed for seafood samples (Rasmussen et al., Anal Bioanal Chem 403:2825–2834, 2012) and has in the present work been tailored for rice products and further optimised for a higher sample throughput and a lower detection limit. Water bath heating (90 °C, 60 min) of samples with dilute HNO3 and H2O2 solubilised and oxidised all iAs to arsenate (AsV). Loading of buffered sample extracts (pH 6 ± 1) followed by selective elution of arsenate from a strong anion exchange SPE cartridge enabled the selective iAs quantification by HG-AAS, measuring total arsenic (As) in the SPE eluate. The in-house validation gave mean recoveries of 101–106 % for spiked rice samples and in two reference samples. The limit of detection was 0.02 mg kg−1, and repeatability and intra-laboratory reproducibility were less than 6 and 9 %, respectively. The SPE HG-AAS method produced similar results compared to parallel high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (ICP-MS) analysis. The SPE separation step was tested collaboratively, where the laboratories (N = 10) used either HG-AAS or ICP-MS for iAs determination in a wholemeal rice powder. The trial gave satisfactory results (HorRat value of 1.6) and did not reveal significant difference (t test, p > 0.05) between HG-AAS and ICP-MS quantification. The iAs concentration in 36 rice samples purchased on the Danish retail market varied (0.03–0.60 mg kg−1), with the highest concentration found in a red rice sample.
Type:
Journal article
Language:
English
Published in:
Analytical and Bioanalytical Chemistry, 2013, Vol 405, Issue 24, p. 7851-7857
Keywords:
Inorganic arsenic; Rice samples; SPE-HG-AAS; Water bath ectraction; Food control; Speciation
Main Research Area:
Science/technology
Publication Status:
Published
Review type:
Peer Review
Submission year:
2013
Scientific Level:
Scientific
ID:
245321772

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