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Liquid–liquid–liquid microextraction followed by HPLC with UV detection for quantitation of ephedrine in urine
Author(s) -
Bagheri Habib,
Khalilian Faezeh,
Ahangar Laleh Enayati
Publication year - 2008
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.200800193
Subject(s) - chromatography , ephedrine , chemistry , high performance liquid chromatography , analyte , extraction (chemistry) , calibration curve , urine , detection limit , liquid–liquid extraction , sample preparation , neuroscience , biology , biochemistry
Liquid–liquid–liquid microextraction (LLLME) in combination with HPLC and UV detection has been used as a sensitive method for the determination of ephedrine in urine samples. Extraction process was performed in a homemade total glass vial without using a Teflon ring, usually employed. Ephedrine was first extracted from 3.5 mL of urine sample (pH 12) into a microfilm of toluene/benzene (50:50). The analyte was subsequently back extracted into an acidic microdrop solution (pH 2) suspended in the organic phase. The extract was then injected into the HPLC system directly. An enrichment factor of 137 along with a good sample clean‐up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 0.01–50 mg/L with regression coefficient corresponding to 0.998. The LODs and LOQs, based on a S/N of 3 and 10, were 5 and 10 μg/L, respectively. The method was eventually applied for the determination of ephedrine in urine sample after oral administration of 5 mg single dose of drug.