Improved analytical approach based on QuECHERS/UHPLC-PDA for quantification of fluoxetine, clomipramine and their active metabolites in human urine samples

Alves, Vera; Conceição, Carlota; Gonçalves, João; Teixeira, Helena M.; Câmara, José

http://hdl.handle.net/10400.13/2508

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Abstract(s)

This paper reports, for the first time, the development of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) combined with a dispersive SPE (d-SPE) based clean-up procedure as a new and powerful strategy for the simultaneous and efficient isolation of two different antidepressants, fluoxetine and clomipramine, and their active metabolites in human urine samples. A univariate experimental design with four independent variables such as sample volume, extraction solvent, buffered salts and clean-up step, was performed and used to investigate the effect of process variables on the extraction efficiency. Good linearity was achieved at the studied concentration range (0.1-5.0 µg mL-1), with correlation coefficients (R2) higher than 0.9961. Low detection limits, ranging between 0.060 and 0.092 μg mL-1 were obtained for all analytes, whereas the lowest quantification limit was 0.1 μg mL-1, corresponding to the lowest concentration of the standard curve. The method also showed good results for accuracy, with values ranging from 91% to 105%. Intra- and inter-day precision, expressed as the relative standard deviation (RSD), were also satisfactory (<10%). Consistent recoveries of antidepressants ranging from 86% to 109% were observed when urine samples were fortified at three concentrations, namely 0.1, 2.5 and 5.0 μg mL-1 In order to evaluate the proposed method for clinical use, the QuEChERS/UHPLC-PDA method was applied to analysis of 12 urine samples from depressed patients.

Keywords

Antidepressive agents Calibration Clomipramine Fluoxetine Limit of detection Mass spectrometry Reproducibility of results QuECHERS/UHPLC-PDA . Faculdade de Ciências Exatas e da Engenharia Centro de Química da Madeira

URI

http://hdl.handle.net/10400.13/2508

Citation

Alves, V., Conceição, C., Gonçalves, J., Teixeira, H. M., & Câmara, J. S. (2017). Improved analytical approach based on QuECHERS/UHPLC-PDA for quantification of fluoxetine, clomipramine and their active metabolites in human urine samples. Journal of analytical toxicology, 41(1), 45-53.