Abstract
Fully-automated magnetic stirring-assisted lab-in-syringe dispersive liquid-liquid microextraction (MAS-LIS-DLLME), combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed for the fast and efficient separation and preconcentration of trace levels of inorganic arsenic species in rice samples. This totally automated analytical procedure combines the advantages of lab-in-syringe flow system and dispersive liquid-liquid microextraction (DLLME) aiming at separation of trace arsenite and arsenate species from natural matrix for the first time. With a single syringe pump that is coupled with a multiposition valve, the whole lab-in-syringe microextraction process including cleaning, mixing, microextraction, phase separation, and target analyte collection was implemented in a fully-automated way. Significant factors of the MAS-LIS-DLLME method were sample acidity, concentration of the chelating agent, amounts of ionic liquids (ILs), aspiration speed and matrix interference. Using the present method, the limits of detection (LODs) for As(v) was 0.005 μg L(-1). The relative standard deviation (RSDs) for seven replicate measurements of 2.0 μg L(-1) of As(v) was 3.7%. The linear dynamic range (LDR) was 0.04-5.0 μg L(-1) and the determination coefficients was 0.9990. Under the optimum conditions, the developed totally automated analytical procedure was successfully applied for the trace arsenite and arsenate species studies in natural rice samples and standard reference materials with satisfactory results.