Determination of arsenic species in rice samples using CPE and ETAAS

A highly sensitive and selective procedure for the determination of arsenate and total arsenic in food by electrothermal atomic absorption spectrometry after cloud point extraction (ETAAS/CPE) was developed. The procedure is based on the formation of a complex of As(V) ions with molybdate in the presence of 50.0 mmol L(-1) sulfuric acid. The complex was extracted into the surfactant-rich phase of 0.06% (w/v) Triton X-114. The variables affecting the complex formation, extraction and phase separation were optimized using factorial designs. Under the optimal conditions, the calibration graph was linear in the range of 0.05-10.0 μg L(-1). The detection and quantification limits were 10 and 33 ng L(-1), respectively and the corresponding value for the relative standard deviation for 10 replicates was below 5%. Recovery values of between 90.8% and 113.1% were obtained for spiked samples. The accuracy of the method was evaluated by comparison with the results obtained for the analysis of a rice flour sample (certified material IRMM-804) and no significant difference at the 95% confidence level was observed. The method was successfully applied to the determination of As(V) and total arsenic in rice samples.