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Simultaneous separation of nitrofuran antibiotics and their metabolites by using micellar electrokinetic capillary chromatography


Wickramanayake, PU and Tran, TC and Hughes, JG and Macka, M and Simpson, N and Marriott, PJ, Simultaneous separation of nitrofuran antibiotics and their metabolites by using micellar electrokinetic capillary chromatography, Electrophoresis, 27, (20) pp. 4069-4077. ISSN 0173-0835 (2006) [Refereed Article]

DOI: doi:10.1002/elps.200600105


Mixtures comprising nitrofuran antibiotics (NFA) and nitrofuran metabolites (NFM) were resolved for the first time by using MEKC. Sodium deoxycholate (SDC) was chosen as the micelle-forming surfactant. Optimization of separation conditions was achieved by using a central composite experimental design (CCD) approach. Experimental parameters such as concentration ratio of borate to phosphate in the buffer, pH of the running electrolyte and voltage were investigated. The effect of concentration of the surfactant on resolution was significant. Under optimal conditions of 80 mM SDC, pH 9.0, (20 mM borate + 20 mM phosphate) and 16 kV, the resolution between eight consecutive peak pairs ranged from 1.9 to 11.8. Due to the absence of a UV-active chromophore in the metabolites, they were derivatized with 2-nitrobenzaldehyde (2-NBA). In order to mimic a proposed extraction procedure for the analysis of both NFA and/or derivatized NFM in a sample, aqueous samples (prederivatized with 2-NBA) were extracted by using C-18 SPE cartridges. After washing with H2O, the cartridges were eluted with a small portion of organic solvent with weak elution characteristics to remove excess 2-NBA (hexane was chosen). Target analytes were then recovered with ACN. Excellent reproducibility of migration time (t(mig)) was achieved for all analytes using the developed MECC approach, with absolute t(mig) < 1 % RSD and t(mig) ratio < 0.2% RSD, and peak area ratio was 4% RSD. The LOD for each compound, calculated by extrapolating to an S/N of 3, were found to be 0.19-2.0 mu g/mL.

Item Details

Item Type:Refereed Article
Keywords:chromatographic exponential function; derivatization; micellar electrokinetic chromatography; nitrofuran antibiotics; nitrofuran metabolites
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Macka, M (Professor Mirek Macka)
ID Code:71610
Year Published:2006
Web of Science® Times Cited:23
Deposited By:Research Division
Deposited On:2011-07-25
Last Modified:2011-07-25

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