An improved analytical strategy combining microextraction by packed sorbent combined with ultra high pressure liquid chromatography for the determination of fluoxetine, clomipramine and their active metabolites in human urine

作者：Alves Vera; Goncalves Joao; Conceicao Carlota; Teixeira Helena M; Camara Jose S^*

来源：Journal of Chromatography A, 2015, 1408: 30-40.

DOI：10.1016/j.chroma.2015.07.021

• Antidepressants
• Human urine samples
• Microextraction by packed sorbent (MEPS)
• Ultra high performance liquid chromatography (UHPLC)

A powerful and sensitive method, by microextraction packed sorbent (MEPS), and ultra-high performance liquid chromatography (UHPLC) with a photodiode array (PDA) detection, is described for the determination of fluoxetine, clomipramine and their active metabolites in human urine samples. The MEPS variables, such as sample volume, pH, number of extraction cycles (draw-eject), and desorption conditions (solvent and solvent volume of elution) were optimized. The analysis were carried out using small sample volumes (500 mu L) and in a short time period (5 min for the entire sample preparation step). Good linearity was obtained for all antidepressants with the correlation coefficients (R-2) above 0.9965. The limits of detection (LOD) ranged from 0.068 to 0.087 mu g mL(-1). The recoveries were from 93% to 98%, with relative standard deviations less than 6%. The inter-day precision, expressed as the relative standard deviation, varied between 3.8% and 8.5% while the intra-day precision between 3.0% and 7.1%. In order to evaluate the proposed method for clinical use, the MEPS/UHPLC-PDA method was applied to analysis of urine samples from depressed patients.

• 出版日期2015-8-21