A simple, inexpensive and efficient method was used for extraction and determination of Fexofenadine and Levocetirizine with three–phase hollow fiber liquid-phase microextraction and high-performance liquid chromatography. Several parameters influencing the extraction recoveries such as the nature of organic extraction solvent, pH of donor and acceptor phases, stirring rate, e xtraction time and salt addition to the sample solution (donor phase) were investigated and optimized. Under the optimized conditions (toluene as organic solvent, pHdonor = 2.5, pHacceptor= 12.0, stirring rate of 1000 rpm, extraction time of 30 min, with no salt addition), extraction recoveries were 64% for Fexofenadine and 79% for Levocetirizine. A good clean-up sample with excellent linearities in the range of 1–500 ng/mL for Fexofenadine (R2=0.997) and 0.6-600 ng/ml for Levocetirizine (R2=0.998) were obtained. The limits of detection were 0.3 ng/mL for Fexofenadine and 0.2 ng/mL for Levocetirizine.
