Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs

In the present work, cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) method was developed and applied for enantioseparation of three imidazole drugs and vinpocetine. The three imidazole drugs namely tioconazole, isoconazole and fenticonazole were simultaneously separated for t...

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Main Author:	Abd. Wahib, Siti Munirah
Format:	Thesis
Language:	English
Published:	2012
Subjects:	Q Science (General)
Online Access:	http://eprints.utm.my/id/eprint/37818/1/SitiMunirahAbd.WahibMFS2012.pdf
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id	my-utm-ep.37818
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spelling	my-utm-ep.378182017-09-25T05:35:16Z Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs 2012-10 Abd. Wahib, Siti Munirah Q Science (General) In the present work, cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) method was developed and applied for enantioseparation of three imidazole drugs and vinpocetine. The three imidazole drugs namely tioconazole, isoconazole and fenticonazole were simultaneously separated for the first time by MEKC technique using dual cyclodextrin (CD) approach. A combination of two neutral CDs; 2-hydroxypropyl-�-CD (HP-�-CD) and heptakis (2,6-di-O-methyl)-�-CD (DM-�-CD) (35 mM: 10 mM) in background electrolyte (BGE) containing 35 mM phosphate buffer (pH 7.0), 50 mM sodium dodecyl sulfate (SDS) and 15% (v/v) acetonitrile at 27 kV and 30oC gave the best separation of six stereoisomers of imidazole drugs with resolutions, Rs 1.90-27.22 and peak efficiencies, N > 180 000 in less than 15 min. The samples were injected electrokinetically at 3 kV for 3 s and detection was carried out at 200 nm. The method was linear over the concentration range of 25-200 mg/L (r2 > 0.998) and the detection limits (S/N = 3) of the three imidazole drugs were found to be 2.7-7.7 mg/L. The CD-MEKC method was successfully applied to the determination of the three imidazole drugs in spiked human urine to give mean recoveries ranging from 72.3 to 107.5% (RSD < 6%, n = 3). The method was also applied to the analysis of commercial cream formulation of tioconazole and isoconazole. Good mean recoveries were obtained, ranging from 93.6-100% (RSD < 7%, n = 3). The best chiral separation of vinpocetine that gave four resolved peaks was achieved using 40 mM HP-�-CD in 50 mM phosphate buffer (pH 7.0) consisting of 40 mM SDS and 10% v/v acetonitrile at a separation temperature of 25oC and separation voltage 25 kV. Samples were injected electrokinetically at 5 kV for 7 s. Vinpocetine detection was accomplished using diode array detector at 200 nm. The complete vinpocetine separation was achieved in less than 15 min with peak resolution, Rs 1.40-5.80. 2012-10 Thesis http://eprints.utm.my/id/eprint/37818/ http://eprints.utm.my/id/eprint/37818/1/SitiMunirahAbd.WahibMFS2012.pdf application/pdf en public masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	Q Science (General)
spellingShingle	Q Science (General) Abd. Wahib, Siti Munirah Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
description	In the present work, cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) method was developed and applied for enantioseparation of three imidazole drugs and vinpocetine. The three imidazole drugs namely tioconazole, isoconazole and fenticonazole were simultaneously separated for the first time by MEKC technique using dual cyclodextrin (CD) approach. A combination of two neutral CDs; 2-hydroxypropyl-�-CD (HP-�-CD) and heptakis (2,6-di-O-methyl)-�-CD (DM-�-CD) (35 mM: 10 mM) in background electrolyte (BGE) containing 35 mM phosphate buffer (pH 7.0), 50 mM sodium dodecyl sulfate (SDS) and 15% (v/v) acetonitrile at 27 kV and 30oC gave the best separation of six stereoisomers of imidazole drugs with resolutions, Rs 1.90-27.22 and peak efficiencies, N > 180 000 in less than 15 min. The samples were injected electrokinetically at 3 kV for 3 s and detection was carried out at 200 nm. The method was linear over the concentration range of 25-200 mg/L (r2 > 0.998) and the detection limits (S/N = 3) of the three imidazole drugs were found to be 2.7-7.7 mg/L. The CD-MEKC method was successfully applied to the determination of the three imidazole drugs in spiked human urine to give mean recoveries ranging from 72.3 to 107.5% (RSD < 6%, n = 3). The method was also applied to the analysis of commercial cream formulation of tioconazole and isoconazole. Good mean recoveries were obtained, ranging from 93.6-100% (RSD < 7%, n = 3). The best chiral separation of vinpocetine that gave four resolved peaks was achieved using 40 mM HP-�-CD in 50 mM phosphate buffer (pH 7.0) consisting of 40 mM SDS and 10% v/v acetonitrile at a separation temperature of 25oC and separation voltage 25 kV. Samples were injected electrokinetically at 5 kV for 7 s. Vinpocetine detection was accomplished using diode array detector at 200 nm. The complete vinpocetine separation was achieved in less than 15 min with peak resolution, Rs 1.40-5.80.
format	Thesis
qualification_level	Master's degree
author	Abd. Wahib, Siti Munirah
author_facet	Abd. Wahib, Siti Munirah
author_sort	Abd. Wahib, Siti Munirah
title	Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
title_short	Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
title_full	Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
title_fullStr	Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
title_full_unstemmed	Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
title_sort	cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2012
url	http://eprints.utm.my/id/eprint/37818/1/SitiMunirahAbd.WahibMFS2012.pdf
_version_	1747816506674118656

Cyclodextrin-modified micellar electrokinetic chromatography for the enantioseparation of imidazole and vinpocetine drugs

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