Sweeping technique combined with micellar electrokinetic chromatography for the simultaneous determination of flunitrazepam and its major metabolites

A sweeping technique, in conjunction with micellar electrokinetic chromatography, for the simultaneous determination of flunitrazepam and its major metabolites, 7-aminoflunitrazepam and N-desmethylflunitrazepam, is described. The optimized conditions for the sweeping and separation were a pH 9.5 buf...

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Bibliographic Details
Published in:Journal of Chromatography A 2006-03, Vol.1110 (1), p.240-244
Main Authors: Huang, Chiung-Wei, Jen, Hsiu-Ping, Wang, Ren-De, Hsieh, You-Zung
Format: Article
Language:English
Subjects:
Analysis
Anti-Anxiety Agents - analysis
Biological and medical sciences
Buffers
Calibration
Cetrimonium Compounds
Cetyltrimethylammonium bromide
Chromatography, Micellar Electrokinetic Capillary - methods
Flunitrazepam
Flunitrazepam - analogs & derivatives
Flunitrazepam - analysis
General pharmacology
Humans
Hydrogen-Ion Concentration
Medical sciences
Micellar electrokinetic chromatography
Pharmacology. Drug treatments
Reproducibility of Results
Sensitivity and Specificity
Sweeping
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Summary:A sweeping technique, in conjunction with micellar electrokinetic chromatography, for the simultaneous determination of flunitrazepam and its major metabolites, 7-aminoflunitrazepam and N-desmethylflunitrazepam, is described. The optimized conditions for the sweeping and separation were a pH 9.5 buffer, 25 mM borate, 50 mM cetyltrimethylammonium bromide, 30% MeOH (v/v), and a 151-mm injection length. The calibration functions were all linear with the coefficient of determination ( r 2) exceeding 0.996 for the three target compounds. Using the sweeping procedure, the limits of detection were determined to be 13.4, 5.6, and 12.0 ng/mL for flunitrazepam, 7-aminoflunitrazepam, and N-desmethylflunitrazepam, respectively, and the sensitivity enhancement for each compound was within the range of 110–200 fold. The RSDs for the retention time and the peak area were less than 4.10%. The optimized sweeping method was also used to examine a spiked urine sample. We conclude that sweeping with micellar electrokinetic chromatography has considerable potential use in clinical and forensic analyses of flunitrazepam and its metabolites.
ISSN:0021-9673
DOI:10.1016/j.chroma.2006.01.070