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2009Dispersive liquid–liquid microextraction using.pdf

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2009Dispersive liquid–liquid microextraction using

J. Sep. Sci. 2009, 32, 3191–3200 M. A. Farajzadeh et al. 3191 Mir Ali Farajzadeh1 Seyed Esmaeil Seyedi1 Mohammad Safi Shalamzari2 Mehdi Bamorowat3 1Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran 2Research and Service Laboratory, Faculty of Chemistry, University of Tabriz, Tabriz, Iran 3GYAH Corporation, Garmdarreh, Tehran, Iran Original Paper Dispersive liquid–liquidmicroextraction using extraction solvent lighter thanwater For the first time a dispersive liquid–liquid microextraction method on the basis of an extraction solvent lighter than water was presented in this study. Three organo- phosphorus pesticides (OPPs) were selected as model compounds and the proposed method was carried out for their preconcentration from water samples. In this extraction method, a mixture of cyclohexane (extraction solvent) and acetone (dis- perser) is rapidly injected into the aqueous sample in a special vessel (see experimen- tal section) by syringe. Thereby, a cloudy solution is formed. In this step, the OPPs are extracted into the fine droplets of cyclohexane dispersed into aqueous phase. After centrifuging the fine droplets of cyclohexane are collected on the upper of the extraction vessel. The upper phase (0.40 lL) is injected into the gas chromatograph (GC) for separation. Analytes were detected by a flame ionization detector (FID) (for high concentrations) or MS (for low concentrations). Some important parameters, such as the kind of extraction and dispersive solvents and volume of them, extrac- tion time, temperature, and salt amount were investigated. Under the optimum conditions, the enrichment factors (EFs) ranged from 100 to 150 and extraction recoveries varied between 68 and 105%, both of which are relatively high over those of published methods. The linear ranges were wide (10–100000 lg/L for GC-FID and 0.01–1 lg/L for GC-MS) and LODs were low (3–4 lg/L for GC-FID and 0.003 lg/L for GC-MS). The RSDs for 100.0 lg/L of each