Liquid-liquid-liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis

Stig Pedersen-Bjergaard*, Knut Einar Rasmussen

*Corresponding author for this work
    1073 Citations (Scopus)

    Abstract

    Methamphetamine as a model compound was extracted from 2.5-mL aqueous samples adjusted to pH 13 (donor solution) through a thin phase of 1-octanol inside the pores of a polypropylene hollow fiber and finally into a 25-μL acidic acceptor solution inside the hollow fiber. Following this liquid- liquid-liquid microextraction (LLLME), the acceptor solutions were analyzed by capillary zone electrophoresis (CE). Extractions were performed in simple disposable devices each consisting of a conventional 4-mL sample vial, two needles for introduction and collection of the acceptor solution, and a 8-cm piece of a porous polypropylene hollow fiber. From 5 to 20 different samples were extracted in parallel for 45 min, providing a high sample capacity. Methamphetamine was preconcentrated by a factor of 75 from aqueous standard solutions, human urine, and human plasma utilizing 10-1 M HCl as the acceptor phase and 10-1 M NaOH in the donor solution. In addition to preconcentration, LLLME also served as a technique for sample cleanup since large molecules, acidic compounds, and neutral components were not extracted into the acceptor phase. Utilizing diphenhydramine hydrochloride as internal standard, repetitive extractions varied less than 5.2% RSD (n = 6), while the calibration curve for methamphetamine was linear within the range 20 ng/μL to 10 μg/mL (r = 0.9983). The detection limit of methamphetamine utilizing LLLME/CE was 5 ng/mL (S/N = 3) in both human urine and plasma.

    Original languageEnglish
    JournalAnalytical Chemistry
    Volume71
    Issue number14
    Pages (from-to)2650-2656
    Number of pages7
    ISSN0003-2700
    DOIs
    Publication statusPublished - 15 Jul 1999

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