Document Type

Journal Article

Department/Unit

Department of Chemistry

Title

Coupling of acetonitrile deproteinization and salting-out extraction with acetonitrile stacking in chiral capillary electrophoresis for the determination of warfarin enantiomers

Language

English

Abstract

Concurrent sample clean-up and enhancement in detection sensitivity for chiral capillary electrophoresis was demonstrated based on the coupling of salting-out extraction with acetonitrile stacking and the use of dimethyl-beta-cyclodextrin as the chiral selector for the sensitive and enantioselective separation of warfarin enantiomers in urine samples. By optimizing the pH of salting-out extraction, warfarin enantiomers can be efficiently extracted from the aqueous sample solution into a smaller volume organic solvent (acetonitrile) phase. The pressure injection of the enriched acetonitrile phase (containing ca. 1% NaCl) into the CE capillary at 10% capillary volume resulted in additional concentration of the warfarin enantiomers. The limit of detection for both warfarin enantiomers was as low as 1.5. ng/mL in urine sample. Our results show that the novel strategy offers improved sensitivity compared to conventional CE analysis, reaching a combined enrichment factor higher than 1000. Calibration curves of warfarin enantiomers in urine samples were found to be linear between 10 and 1000. ng/mL, and intra- and inter-day precision (N= 9) for both warfarin enantiomers in terms of migration time and peak area were found to be within the range of 0.1-0.8% and 1.0-6.7%, respectively. The recovery of warfarin enantiomers from urine was ca. 90%. © 2011 Elsevier B.V.

Keywords

Acetonitrile deproteinization, Acetonitrile stacking, Chiral capillary electrophoresis, Salting-out extraction

Publication Date

2011

Source Publication Title

Journal of Chromatography A

Volume

1218

Issue

26

Start Page

4045

End Page

4051

Publisher

Elsevier

DOI

10.1016/j.chroma.2011.04.067

ISSN (print)

00219673

ISSN (electronic)

18733778

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