title: Determination and Uncertainty Analysis of Inorganic Arsenic in Husked Rice by Solid Phase Extraction and Atomic Absorption Spectrometry with Hydride Generation.
abstract: This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were <2, meeting the performance criteria mandated by the EC. The combined standard measurement uncertainty by this method was less than the maximum standard measurement uncertainty; thus, the method can be considered for official control purposes. The method was applied for the determination of iAs in husked rice samples and has potential applications in other food commodities.
authors.affiliation: Export Inspection Council of India, New Delhi YMCA Cultural Centre Building, 3rd Floor, 1 Jai Singh Rd, New Delhi 110 001, India.
authors.forename: Sushil Kumar
authors.initials: SK
authors.lastname: Saxena
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Agnes Raju
authors.initials: AR
authors.lastname: Karipalli
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Anoop A
authors.initials: AA
authors.lastname: Krishnan
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Rajesh
authors.initials: R
authors.lastname: Rangasamy
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Praveen
authors.initials: P
authors.lastname: Malekadi
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Dhirendra P
authors.initials: DP
authors.lastname: Singh
authors.affiliation: Export Inspection Agency - Kolkata Laboratory, 101 Southend Conclave, 1582 Rajdanga Main Rd, Kolkata 700 107, India.
authors.forename: Vimesh
authors.initials: V
authors.lastname: Vasu
authors.affiliation: Export Inspection Agency - Kolkata, World Trade Centre, 14/1B Ezra St, Kolkata 700 001, India.
authors.forename: Vijay K
authors.initials: VK
authors.lastname: Singh
mesh_terms: D001151:Arsenic / Q000032:analysis*; D005504:Food Analysis; D006861:Hydrogen Peroxide; D012275:Oryza / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D013054:Spectrophotometry, Atomic; D035501:Uncertainty
chemical_list: D006861:Hydrogen Peroxide; D001151:Arsenic