Speciation of Fe(II) and Fe(III) in Chinese Yellow Rice Wine Using Direct Immersion Dual-Drop Microextraction Coupled with Graphite Furnace Atomic Absorption Spectrometry (GFAAS)

A new direct immersion dual-drop microextraction (DIDDME) procedure is described for Fe(III) and Fe(II) speciation followed by detection with graphite furnace atomic absorption spectrometry. This method is based upon the selective reaction of 1-(2-pyridylazo)-2-naphthol (PAN) and N-benzoyl-N-phenylhydroxylamine (BPHA) with Fe(II) and Fe(III) to form complexes at pH 1.5. Two solvent drops that contain PAN and BPHA were concurrently immersed in a sample solution for simultaneous separation of Fe(III) and Fe(II), respectively. This method eliminated time-consuming and labor-intensive oxidation of Fe(II) or reduction of Fe(III), which may provide incomplete conversion and contamination. Using the optimal conditions, the detection limits were 0.067 ng mL(-1) and 0.054 ng mL(-1) for Fe(II) and Fe(III) with relative standard deviations of 6.0% and 5.1%, respectively. Enrichment factors of 300-fold were obtained. The procedure was successfully utilized for the determination of Fe(II) and Fe(III) in Chinese yellow wine. To evaluate accuracy of this method, a rice certified reference material was analyzed and the result was in good agreement with the certified value.