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The current non-chromatographic speciation methods generally involve the conversion of different species by oxidation/reduction reactions, which may cause inherent problems such as contamination risk, time consumption and complex operations. In this work, in-syringe solid phase extraction (IS-SPE) was combined with in-syringe vortex-assisted solidified floating organic drop microextraction (IS-VA-SFODME) for the detection of Sb(V) and Sb(III) in rice wines by graphite furnace atomic absorption spectrometry. Firstly, IS-SPE involved the use of ZnFe 2 O 4  nanotubes as the sorbent for the isolation and enrichment of Sb(V) and removal of the matrix components such as ethanol, pigment, sugars and carbohydrates. Then, IS-VA-SFODME was used for enriching Sb(III) in the original sample solution after IS-SPE. This technique exhibited good anti-interference ability and high enrichment efficiency without tedious pre-oxidation/pre-reduction and centrifugation/filtration operations, which may cause the contamination of samples. Under the selected conditions, the detection limits were 4.5 ng L −1  and 3.2 ng L −1  for Sb(III) and Sb(V) with relative standard deviations of 7.3% and 5.1%, respectively. This procedure was used with satisfactory results for the detection of Sb(III) and Sb(V) in rice wine samples and a certified reference material of water sample. Recoveries of spiked experiments ranged from 91.0 to 107%.

food additives and contaminants: part a

In-syringe solid phase extraction and in-syringe vortex-assisted solidified floating organic drop microextraction of Sb(III) and Sb(V) in rice wines with determination by graphite furnace atomic absorption spectrometry