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In this work, extraction of volatile compound in thymus essential oil and fruit juice samples was followed using coacervative microextraction technique by gas chromatography with flame ionization detection (GC-FID). Oleic acid (10 pL) was dissolved in THF (3.5 mL) in 10 mL volumetric flask. Aqueous sample (6.5 mL) containing analytes and internal standard was added to give a final volume of 10 mL. The coacervate formed instantaneously, two phases were separated by centrifugation. The analytes in the coacervate phase was determined by the gas chromatograph. The influence of several important parameters on extraction efficiency was evaluated. Under optimized experimental conditions, the calibration graphs were linear in the range of 0.5–30.0 mg/L with coefficient of determination more than 0.994 for all analytes. The limits of detection values were in the range of 0.13–0.31 mg/L. The limit of quantification …