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Ultrasound‐assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid–liquid microextraction
Author(s) -
Alshana Usama,
Göğer Nilgün G.,
Ertaş Nusret
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200308
Subject(s) - chromatography , capillary electrophoresis , disperser , chemistry , extraction (chemistry) , solid phase microextraction , detection limit , pseudoephedrine , ephedrine , sample preparation , analyte , liquid liquid , analytical chemistry (journal) , materials science , gas chromatography–mass spectrometry , mass spectrometry , neuroscience , composite material , biology
Ultrasound‐assisted emulsification microextraction and dispersive liquid–liquid microextraction were compared for extraction of ephedrine, norephedrine, and pseudoephedrine from human urine samples prior to their determination by capillary electrophoresis. Formation of a microemulsion of the organic extract with an aqueous solution (at p H 3.2) containing 10% methanol facilitated the direct injection of the final extract into the capillary. Influential parameters affecting extraction efficiency were systematically studied and optimized. In order to enhance the sensitivity further, field‐amplified sample injection was applied. Under optimum extraction and stacking conditions, enrichment factors of up to 140 and 1750 as compared to conventional capillary zone electrophoresis were obtained resulting in limits of detection of 12–33 μg/ L and 1.0–2.8 μg/ L with dispersive liquid–liquid microextraction and ultrasound‐assisted emulsification microextraction when combined with field‐amplified sample injection. Calibration graphs showed good linearity for urine samples by both methods with coefficients of determination higher than 0.9973 and percent relative standard deviations of the analyses in the range of 3.4–8.2% for ( n = 5). The results showed that the use of ultrasound to assist microextraction provided higher extraction efficiencies than disperser solvents, regarding the hydrophilic nature of the investigated analytes.