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In this study, homogeneous liquid–liquid microextraction (HLLME) was developed for preconcentration and extraction of 15 organophosphorus pesticides (OPPs) from water samples coupling with gas chromatography followed by a flame photometric detector (HLLME-GC-FPD). In this method, OPPs were extracted by the homogeneous phase in a ternary solvent system (water/acetic acid/chloroform). The homogeneous solution was excluded by the addition of sodium hydroxide as a phase separator reagent and a cloudy solution was formed. After centrifugation (3 min at 5,000 rpm), the fine particles of extraction solvent (chloroform) were sedimented at the bottom of the conical test tube (10.0 ± 0.5 µL). Furthermore, 0.5 µL of the sedimented phase was injected into the GC for separation and determination of OPPs. Optimal results were obtained under the following conditions: volume of the extracting solvent (chloroform), 53 µL; volume of the consolute solvent (acetic acid), 0.76 mL and concentration of sodium hydroxide, 40% (w/v). Under the optimum conditions, the enrichment factors of (260–665), the extraction percent of 75.8–104%, the dynamic linear range of 0.03–300 µg L −1  and the limits of detection of 0.004–0.03 µg L −1  were obtained for the OPPs. This method was successfully applied for the extraction and determination of the OPPs in environmental water samples.

journal of chromatographic science

Homogeneous Liquid–Liquid Microextraction for Determination of Organophosphorus Pesticides in Environmental Water Samples Prior to Gas Chromatography-Flame Photometric Detection