In this thesis, the combination of liquid-liquid micro-extraction method with diffusive thin film was used to extract rivastigmine (as the target compound) and identified by ion mobility spectroscopy with secondary electrospray ionization source. The film used in this method was prepared using electrospinning method. To measure very small amounts of rivastigmine and achieve the highest extraction efficiency, effective parameters such as type of extracting and dispersing solvents, volume of extracting and dispersing solvents, centrifugation time, solvent evaporation time from the film surface and pH were studied. Type of extraction solvent; Trichloromethane, type of dispersant solvent; methanol, volume of extracting solvent; 90 microliters, spray solvent volume; 1.5 ml, evaporation time from the film surface; 1 minute and centrifuge time; 5 minutes and the pH of the sample solution;10 was obtained. In this method, the detection limit (DL) was 3 ?g/L, the linear range (LR) was 10-1000 ?g/L with a correlation coefficient of 0.9976. The intra- and inter-day relative standard deviations were calculated to be 4% and 6%, respectively. Based on these analytical parameters, the proposed method provides a suitable method with high sensitivity, fast and repeatable and without solvent disturbance for measuring very small amounts of rivastigmine in biological samples such as urine, saliva and plasma.