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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 32, Number 11
BKCSDE 32(11)
November 20, 2011 

Ultra-trace Arsenic Determination in Urine and Whole Blood Samples by Flow Injection-Hydride Generation Atomic Absorption Spectrometry after Preconcentration and Speciation Based on Dispersive Liquid-Liquid Microextraction
Hamid Shirkhanloo, Ahmad Rouhollahi,*, Hassan Zavvar Mousavi
Arsenic, Speciation, Ionic liquid, Dispersive liquid-liquid microextraction, FI-HGAAS
A noble method for pre-concentration and speciation of ultra trace As (III) and As (V) in urine and whole blood samples based on dispersive liquid-liquid microextraction (DLLME) has been developed. In this method, As (III) was complexed with ammonium pyrrolidine dithiocarbamate at pH = 4 and Then, As (III) was extracted into the ionic liquid (IL). Finally, As (III) was back-extracted from the IL with hydrochloric acid (HCl) and its concentration was determined by flow injection coupled with hydride generation atomic absorption spectrometry (FI-HGAAS). Total amount of arsenic was determined by reducing As (V) to As (III) with potassium iodide (KI) and ascorbic acid in HCl solution and then, As (V) was calculated by the subtracting the total arsenic and As (III) content. Under the optimum conditions, for 5-15 mL of blood and urine samples, the detection limit (3σ) and linear range were achieved 5 ng L−1 and 0.02-10 μg L−1, respectively. The method was applied successfully to the speciation and determination of As (III) and As (V) in biological samples of multiple sclerosis patients with suitable precision results (RSD < 5%). Validation of the methodology was performed by the standard reference material (CRM).
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