Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography

Micellar electrokinetic chromatography (MEKC) is increasingly popular in the analysis of organic pollutants in the environment due to its high separation efficiency, less solvent usage and shorter analysis time. In this study, MEKC was used for the separation of 2,3,7,8-tetrachlorodibenzo-p-dioxin (...

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Main Author:	Liew, Sharain Yen Ling
Format:	Thesis
Language:	English
Published:	2007
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/9861/1/SharainLiewYenMFSA2007.pdf
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spelling	my-utm-ep.98612018-07-25T08:00:00Z Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography 2007-12 Liew, Sharain Yen Ling QD Chemistry Micellar electrokinetic chromatography (MEKC) is increasingly popular in the analysis of organic pollutants in the environment due to its high separation efficiency, less solvent usage and shorter analysis time. In this study, MEKC was used for the separation of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 2,3,7,8- tetrachlorodibenzo-p-furan (TCDF) with a separation buffer consisting of 20 mM sodium cholate, 20 mM sodium tetraborate decahydrate and 5% v/v organic modifier acetonitrile-methanol (3:1 v/v) at a final buffering pH of 9.16-9.22. Separation voltage was at 25 kV with anodic injection and optimum wavelength set at 225 nm. To improve the limit of detection (LOD), five on-line preconcentration techniques were evaluated. The techniques were normal stacking mode (NSM-MEKC), reversed electrode polarity stacking mode (REPSM-MEKC), high conductivity sample stacking mode (HCSSM-MEKC), sweeping and field enhanced sample injection (FESI-MEKC). High conductivity sample stacking method-MEKC (HCSSMMEKC) that gave an LOD of 46 ppb for TCDF and 18.5 ppb for TCDD was chosen. Solid phase disc extraction (SPDE) was used to further improve the LOD during the extraction of TCDF and TCDD from water thus reducing the LODs by 1000 fold. LODs in the ppt range were achieved for both analytes. This is the first study conducted using MEKC for 2,3,7,8-TCDF and 2,3,7,8-TCDD. Selected hydrophilic organophosphorous pesticides were also included in this study. They were dicrotophos, monocrotophos and phosphamidon. Separations were carried out using acidic buffer (pH 2.3) with a buffering system consisting of 10 mM sodium dodecyl sulphate, 20 mM sodium dihydrogen phosphate and 10% v/v methanol. Optimum detection wavelength of 225 nm with separation voltage at -25 kV was used. MEKC separation gave LODs of 32.1 ppm for dicrotophos, 3.75 ppm for monocrotophos and 18.6 ppm for phosphamidon. Stacking with reverse migrating micelles (SRMM) gave better LODs of 0.15 ppm for dicrotophos, 0.39 ppm for monocrotophos and 0.22 ppm for phosphamidon. SPDE was able to reduce the LOD further by 250 fold. Sample matrix used was spiked pond water. MEKC was successfully used to separate the test analytes in pond water sample. These analytes consisted of 2,3,7,8- TCDF and 2,3,7,8-TCDD under basic conditions and three hydrophilic organophosphorous pesticides under acidic conditions with analysis time of less than 10 minutes. 2007-12 Thesis http://eprints.utm.my/id/eprint/9861/ http://eprints.utm.my/id/eprint/9861/1/SharainLiewYenMFSA2007.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	QD Chemistry
spellingShingle	QD Chemistry Liew, Sharain Yen Ling Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
description	Micellar electrokinetic chromatography (MEKC) is increasingly popular in the analysis of organic pollutants in the environment due to its high separation efficiency, less solvent usage and shorter analysis time. In this study, MEKC was used for the separation of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 2,3,7,8- tetrachlorodibenzo-p-furan (TCDF) with a separation buffer consisting of 20 mM sodium cholate, 20 mM sodium tetraborate decahydrate and 5% v/v organic modifier acetonitrile-methanol (3:1 v/v) at a final buffering pH of 9.16-9.22. Separation voltage was at 25 kV with anodic injection and optimum wavelength set at 225 nm. To improve the limit of detection (LOD), five on-line preconcentration techniques were evaluated. The techniques were normal stacking mode (NSM-MEKC), reversed electrode polarity stacking mode (REPSM-MEKC), high conductivity sample stacking mode (HCSSM-MEKC), sweeping and field enhanced sample injection (FESI-MEKC). High conductivity sample stacking method-MEKC (HCSSMMEKC) that gave an LOD of 46 ppb for TCDF and 18.5 ppb for TCDD was chosen. Solid phase disc extraction (SPDE) was used to further improve the LOD during the extraction of TCDF and TCDD from water thus reducing the LODs by 1000 fold. LODs in the ppt range were achieved for both analytes. This is the first study conducted using MEKC for 2,3,7,8-TCDF and 2,3,7,8-TCDD. Selected hydrophilic organophosphorous pesticides were also included in this study. They were dicrotophos, monocrotophos and phosphamidon. Separations were carried out using acidic buffer (pH 2.3) with a buffering system consisting of 10 mM sodium dodecyl sulphate, 20 mM sodium dihydrogen phosphate and 10% v/v methanol. Optimum detection wavelength of 225 nm with separation voltage at -25 kV was used. MEKC separation gave LODs of 32.1 ppm for dicrotophos, 3.75 ppm for monocrotophos and 18.6 ppm for phosphamidon. Stacking with reverse migrating micelles (SRMM) gave better LODs of 0.15 ppm for dicrotophos, 0.39 ppm for monocrotophos and 0.22 ppm for phosphamidon. SPDE was able to reduce the LOD further by 250 fold. Sample matrix used was spiked pond water. MEKC was successfully used to separate the test analytes in pond water sample. These analytes consisted of 2,3,7,8- TCDF and 2,3,7,8-TCDD under basic conditions and three hydrophilic organophosphorous pesticides under acidic conditions with analysis time of less than 10 minutes.
format	Thesis
qualification_level	Master's degree
author	Liew, Sharain Yen Ling
author_facet	Liew, Sharain Yen Ling
author_sort	Liew, Sharain Yen Ling
title	Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
title_short	Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
title_full	Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
title_fullStr	Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
title_full_unstemmed	Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
title_sort	analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2007
url	http://eprints.utm.my/id/eprint/9861/1/SharainLiewYenMFSA2007.pdf
_version_	1747814782303469568

Analysis of dioxin and furan related compounds and organophosphorous pesticdes using micellar electrokinetic chromatography

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