In this research, coupling of hollow fiber based liquid–liquid–liquid microextraction (HF-LLLME) method and ESI-IMS was used for preconcentration and determination of Propranolol in biological samples including urine and plasma. For finding better efficiency the three-phase LPME by Acetic Acid acceptor phase and the three-phase LPME by MeOH acceptor phase were be tested. In hollow fiber based liquid–liquid–liquid microextraction, a layer of organic phase is impregnated into the pores of a porous hollow fiber, while the lumen of the hollow fiber was filled with CH3COOH (0.5 M) solution as an acceptor solution that was connected directly to the needle of a microsyringe. The fiber was then immersed into 3 ml of a basic aqueous sample. Effective parameters on HF-LLLME such as solvent type, pH of donor phase, acidity of acceptor phase, sample stirring rate, salt addition, extraction temperature and extraction time were studied. The extraction efficiency of HF-LPME by Acetic Acid Acceptor was achieved utilizing a 1.3 cm porous hollow fiber immobilized with Isoamylbenzoate, 0.001M NaOH, 3 mL donor phase sample, without NaCl addition,0.005M CH3COOH solution as acceptor phase, 1000 rpm stirring rate and 20 min extraction time at room temperature. The analyte was extracted quantitatively from the sample solution into the acceptor solution with an enrichment factor 40. The limit of detection of the method was 1.6 µg/L. Correlation Coefficient was 0.991 and inter and intra relative standard deviation were 6% and 12% respectively. The extraction efficiency of HF-LPME by MeOH Acceptor was achieved utilizing a 4cm porous hollow fiber immobilized with n-dodecane, 0.001M NaOH, 3 mL donor phase sample , without NaCl addition, 0.0005 M CH3COOH solution as acceptor phase, 1200 rpm stirring rate and 15 min extraction time at room temperature. The analyte was extracted quantitatively from the sample solution into the acceptor solution with an enrichment factor 21. The limit of detection of the method was 1.76 µg/L.The Correlation Coefficient was 0.993 and relative standard deviation in a day was 7% and between days was 5%. Results show that microextractions with Acetic acid and MeOH acceptors have same Limit of Detection, linear range. The enrichment factor for acetic acid acceptor was 40 and for MeOH was equal to 21. Not requiringto dilution, MeOH Acceptor is faster.
