Determination of total arsenic and speciation analysis in Mexican maize tortillas by hydride generation - microwave plasma atomic emission spectrometry and high performance liquid chromatography - inductively coupled plasma - mass spectrometry

• Published in: Analytical methods Vol. 9; no. 13; pp. 259 - 268
• Main Authors: Guerrero Esperanza, Moises, Yanez Barrientos, Eunice, Wrobel, Kazimierz, Acevedo Aguilar, Francisco Javier, Corrales Escobosa, Alma Rosa, Wrobel, Katarzyna
• Format: Journal Article
• Language: English
• Published: 07.04.2017
• Subjects: Anion exchanging; Arsenic; Atomic properties; Cartridges; Exchange; Recovery; Spectrometry; Spectroscopy
• ISSN: 1759-9660; 1759-9679
• DOI: 10.1039/c7ay00224f

The determination of total arsenic (tAs), inorganic As (iAs = As( iii ) + As( v )) and As speciation in Mexican maize tortillas has been undertaken for the first time. Hydride generation - microwave plasma atomic emission spectrometry (HG-MP-AES) with tellurium (sodium tellurite Te( iv )) as the internal standard (IS) yielded tAs results in good agreement with those provided by inductively coupled plasma mass spectrometry (ICP-MS). In seven products from local markets, tAs was found in the range of 21.8-192 μg As kg −1 . Analysis of As( iii ), As( v ), MMAs( v ), and DMAs( v ) by an established anion exchange liquid chromatography - ICP-MS procedure showed that iAs corresponded to 72.3-98.0% of tAs. A non-chromatographic procedure was envisioned for iAs: diluted tortilla extract or calibration solution (pH 9.0) was loaded on a strong anion exchange cartridge modified with silver chloride, iAs fraction was collected and analyzed by HG-MP-AES with IS. For tAs by HG-MP-AES (with IS) the method quantification limit was 47.6 μg As kg −1 whereas for iAs it got worse (95 μg As kg −1 ) due to the low recovery of this As form in SPE (<30%). In an attempt to eliminate matrix interference, the lower sample volume was loaded on the cartridge and ICP-MS was used for quantification, yielding an improved percentage recovery of 73.4%. On the other part, the iAs recovery was >93% while analyzing natural water with off-line quantification by any of the two atomic spectrometry techniques, indicating that the chemical matrix of tortillas was responsible for poor SPE performance. It is concluded that HG-MP-AES with IS is a cost-effective alternative for the determination of tAs that offers improved precision under a non-rigorous protocol; however, efficient separation/preconcentration of iAs by SPE is still a challenge. Determination and speciation of As in tortillas are reported.