A method was established for the determination of ciprofloxacin hydrochloride (CIPRO) in the blood serum and pharmaceutical samples by a combination of cloud point extraction with UV-Vis spectrophotometry. The method included the formation of Fe (III) -CIPRO complex in presence of dilute H 2 SO 4 , followed the extraction of the complex by cloud point extraction using non-ionic surfactant Triton X-114. The surfactant phase extracted was dissolved in little amount of solvent and the CIPRO quantity measured spectrophotometerically at absorption maximum of 437 nm. The effect of the experimental factors which affect the CPE efficiency was optimized by classical method. The preconcentration and enrichment factors were found to be 40 and 143 fold respectively, achieving the detection limit of 0.77 µg mL -1 and linear range of 2.5-120 µg mL -1 with correlation coefficient of 0.9984, under the optimum conditions. The average recovery percentage of CIPRO was of 98.89±0.87% and the precision in the range of 1.15-2.85%. The suggested method was applied for the determination of CIPRO in the serum samples of different subjects orally administrated for two hours with Emicipro 500, in addition to drug formulations like UFEXIL ® infusion and Ciprodar ® tablets. The experimental values were agreed with the quoted values that stated by the manufacturer' companies.
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