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Abstract
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tThe purpose of this study is the development and validation of a simple, novel, selective and fast off-linemicroextraction technique combining capillary electrophoresis with in-column field-amplified sampleinjection (FASI) for the simultaneous determination of capecitabine (CAP) and its active metabolite, 5-Fluorouracil (5-FU), in human plasma. At the moment, there is a lack of using cost-effective CE toolcombined with novel miniaturized sample clean-up techniques for analysis of these important anti-cancer agents in plasma samples. This paper intends to fill this gap and describe a simple off-line samplepretreatment by means of AgNPs@MCM-41 reinforced hollow fiber Solid/Liquid phase microextraction(AgNPs@MCM41-HF-SLPME) with subsequent quantitation by FASI-CE. The separation of analytes wasperformed using a BGE containing 60 mM phosphate-Tris buffer (pH 7) with 10% methanol as an organicmodifier. Before sample loading, a short water plug (50 mbar, 3 s) was injected to permit FASI for stack-ing. Various parameters affecting the off-line microextraction efficiency as well as FASI were optimized.Migration time was found to be 6.6 (±0.1) min for 5-FU and 7.4 (±0.2) min for CAP. The linearity, pre-cision, accuracy, recovery, selectivity, specificity, stability as well as the robustness of the method wasevaluated from spiked plasma samples during the course of validation. The results revealed that the pre-sented technique demonstrates acceptable accuracy and precision, miniaturized sample preparation anda reduced need for complicated equipment along with an acceptable analysis time. The validated methodwas successfully applied to determine CAP and 5-FU in patient’s plasma samples.
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