Abstract

The combination of hollow fiber liquid–liquid–liquid microextraction and electrospray ionization-ion mobility spectrometry (ESI-IMS) was used for the analysis of diclofenac in biological samples. Diclofenac was extracted from an acidic aqueous sample into methanol as an acceptor phase, through n-dodecane impregnated in the hollow fiber pores. The extracted drug was detected with ESI-IMS in the negative mode. Extraction parameters including pH of donor phase, stirring rate, sample ionic strength, temperature and extraction time were studied. The linearity of the method for the determination of diclofenac was in the range of 100–2000 and 60–2000 µg L−1 for plasma and urine, respectively. The detection limit of the method was also 34 and 21 µg L−1 in the plasma and urine, respectively. The applicability of the method for analyzing the analyte in biological samples was investigated. The method was also applied to analysis of urine and plasma of a healthy volunteer after oral administration of diclofenac.

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