Determination of arsenic in scalp hair samples from exposed subjects using microwave-assisted digestion with and without enrichment based on cloud point extraction by electrothermal atomic absorption spectrometry

Abstract

A simple and rapid cloud point extraction (CPE) procedure was applied for preconcentration of trace quantities of arsenic (As) in scalp hair samples. The samples were subjected to microwave-assisted digestion in a mixture of nitric acid and hydrogen peroxide (2 + 1, v/v) prior to preconcentration by CPE. The As in digested samples was complexed with ammonium pyrrolidine dithiocarbamate (APDC), and the resultant As-PDC complex was extracted by a nonionic surfactant, octylphenoxypolyethoxyethanol (Triton X-114). After centrifugation, the surfactant-rich phase was diluted with 0.1 M HNO3 in methanol and analyzed by electrothermal atomic absorption spectrometry. The experimental parameters, i.e., amount of APDC, concentration of Triton X-114, equilibrium temperature and time, were optimized. For validation of the proposed method, a certified reference material (CRM) of human hair (BCR 397) was used. No significant difference (P > 0.05) was observed between the experimental results and certified values of the CRM (paired t-test). The LOD and LOQ obtained under the optimal conditions were 0.025 and 0.083 μg/kg, respectively. The developed method was applied for the determination of As in scalp hair samples from male and female subjects of two villages of Khairpur Mir's, Pakistan.