A new preconcentration method termed, homogeneous liquid assistance (HLLME-FA) has been developed method, home-designed extraction cell was used procedure. The novel approach avoids the centrifugation step. In this extraction method, a mixture of toluene (extraction solvent) and acetone (homogeneous sample solution. By using air flotation, the organic Parameters affecting the extraction efficiency such as type and volume of ionic strength and extraction time were studied and optimized. The new method (HLLME limit of 0.1 µg L-1 and calibration graph was linear in the range of 1.0 FA is a suitable method for the determination of Malathion in water samples