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  • Validation of two spectrophotometric methods for fluoxetine quantification
    Publication . Gaspar, Joana; Barbosa Moreira, Zélia
    Objective: This paper describes the development and validation of two UV-Visible spectrophotometric analysis methods, using absolute ethanol (method A) and HCl 0.1 M (method B) as solvents, to quantify fluoxetine (FLX) in its generic and brand name form. The objective is to validate both methods and compare the concentrations of the samples obtained from each one. Methods: Validation of each method with the determination of linearity, limit of detection and quantification, intermediary precision, robustness, accuracy and uniformity of mass for both samples was performed. Results: Uniform distribution of FLX in capsules were verified and good linear relationships were found between the readings and the concentrations of FLX, in the ranges of 100 μg/ml to 300 μg/ml and 5 μg/ml to 25 μg/ml, for method A and B, respectively. The limit of quantification obtained was 9.96 μg/ml for method A and 0.87 μg/ml for method B. The limit of detection obtained was 2.988 μg/ml for method A and 0.26 μg/ml for method B. Was also verified robustness, good inter-day precision and accuracy of both methods. Conclusion: The methods were successfully validated to the determination of FLX in its pharmaceutical formulations.
  • Optimization of a dispersive liquid–liquid microextraction method followed by UHPLC analysis for fluoxetine quantification in environmental water resources
    Publication . Runfola, Massimiliano; Lima, Diana L.D.; Fonseca, Ana; Barbosa Moreira, Zélia
    Fluoxetine is the most prescribed drug for treatment of depression. Recently, its presence in aquatic environment has been receiving a growing interest as several studies assessed its effects on aquatic fauna. Therefore, it's important to have an analytical method capable of monitoring these compounds at low concentrations. In this study, a new method was developed based on dispersive liquid–liquid microextraction to preconcentrate fluoxetine in a small volume of water sample (6 mL) before chromatographic analysis using ultra high performance liquid chromatography with fluorescence detection. Effect of composition and volume of extracting mixture, sample pH, vortexing time and salt addition were evaluated. Optimization of extraction conditions lead to an enrichment factor of 61 ± 18. After extraction optimization, recovery percentages of fluoxetine spiked into different water matrices between 83–110% were obtained. For the optimized method, the calibration curve was obtained in the range of 160–2500 ng/L with a limit of detection of 98.9 ng/L and a limit of quantification of 329.8 ng/L.