Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides

An organic-inorganic hybrid 3-aminopropyltrimethoxysilane (APTMS)- polydimethylsiloxane (PDMS) was produced using sol-gel method and used as coating on glass encased stir bar. The physico-chemical properties and extraction ability of the APTMS/PDMS hybrid coatings were manipulated by varying the mol...

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Main Author:	Hasnan, Zafran
Format:	Thesis
Language:	English
Published:	2012
Subjects:	QD Chemistry RA Public aspects of medicine
Online Access:	http://eprints.utm.my/id/eprint/28397/5/ZafranHasnanMFS2012.pdf
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id	my-utm-ep.28397
record_format	uketd_dc
spelling	my-utm-ep.283972017-09-30T05:50:42Z Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides 2012-07 Hasnan, Zafran QD Chemistry RA Public aspects of medicine An organic-inorganic hybrid 3-aminopropyltrimethoxysilane (APTMS)- polydimethylsiloxane (PDMS) was produced using sol-gel method and used as coating on glass encased stir bar. The physico-chemical properties and extraction ability of the APTMS/PDMS hybrid coatings were manipulated by varying the molar ratio of APTMS to PDMS, amount of water and types of catalysts during sol synthesis. Fourier Transform Infrared Spectroscopy results showed successful hybridization between PDMS and amino moiety. Field Emission Scanning Electron Microscopy showed a homogenous surface image of the APTMS/PDMS hybrid coating while nitrogen adsorption indicated that the hybrid is a mesoporous material (pore size ~2.9 nm). The ability of the APTMS/PDMS hybrid coatings were investigated for stir bar sorptive extraction (SBSE) of two selected organophosphorus pesticides (OPPs) namely polar dicrotophos and mid-polar malathion. Analysis was performed using HPLC with UV detector. Optimized SBSE parameters using APTMS/PDMS hybrid coating were 300 rpm stirring rate, 15 min extraction time, 1 mL methanol as ultrasonic assisted liquid desorption (UA-LD) solvent and 25 min desorption time. The optimized SBSE parameters using PDMS-coated TWISTER were also similar with the APTMS/PDMS hybrid coating except that the stirring rate used was 600 rpm. The limit of detection (LOD) (S/N=3) of dicrotophos is 0.108 mg L-1 and 0.158 mg L-1 for malathion using APTMS/PDMS hybrid coating. LOD (S/N=3) of malathion is 0.31 mg L-1 but dicrotophos was not detected with the PDMS-coated TWISTER. The APTMS/PDMS sol-gel coating developed for SBSE was successfully applied for the determination of OPPs in grape and cucumber samples, and its performance was compared with commercial PDMS TWISTER. The recoveries of dicrotophos and malathion from cucumber and grape samples using APTMS/PDMS hybrid coating was 71% and 98%, respectively with RSD 3.1%-3.6%. The recoveries of malathion in cucumber and grape using PDMS-coated TWISTER was 91% and 62% respectively, with acceptable RSD 7.46%. SBSE using APTMS/PDMS hybrid coating showed better selectivity for the polar dicrotophos compared to commercial PDMS-coated TWISTER, which failed to extract the polar dicrotophos. 2012-07 Thesis http://eprints.utm.my/id/eprint/28397/ http://eprints.utm.my/id/eprint/28397/5/ZafranHasnanMFS2012.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:69660?site_name=Restricted Repository masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	QD Chemistry RA Public aspects of medicine
spellingShingle	QD Chemistry RA Public aspects of medicine Hasnan, Zafran Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
description	An organic-inorganic hybrid 3-aminopropyltrimethoxysilane (APTMS)- polydimethylsiloxane (PDMS) was produced using sol-gel method and used as coating on glass encased stir bar. The physico-chemical properties and extraction ability of the APTMS/PDMS hybrid coatings were manipulated by varying the molar ratio of APTMS to PDMS, amount of water and types of catalysts during sol synthesis. Fourier Transform Infrared Spectroscopy results showed successful hybridization between PDMS and amino moiety. Field Emission Scanning Electron Microscopy showed a homogenous surface image of the APTMS/PDMS hybrid coating while nitrogen adsorption indicated that the hybrid is a mesoporous material (pore size ~2.9 nm). The ability of the APTMS/PDMS hybrid coatings were investigated for stir bar sorptive extraction (SBSE) of two selected organophosphorus pesticides (OPPs) namely polar dicrotophos and mid-polar malathion. Analysis was performed using HPLC with UV detector. Optimized SBSE parameters using APTMS/PDMS hybrid coating were 300 rpm stirring rate, 15 min extraction time, 1 mL methanol as ultrasonic assisted liquid desorption (UA-LD) solvent and 25 min desorption time. The optimized SBSE parameters using PDMS-coated TWISTER were also similar with the APTMS/PDMS hybrid coating except that the stirring rate used was 600 rpm. The limit of detection (LOD) (S/N=3) of dicrotophos is 0.108 mg L-1 and 0.158 mg L-1 for malathion using APTMS/PDMS hybrid coating. LOD (S/N=3) of malathion is 0.31 mg L-1 but dicrotophos was not detected with the PDMS-coated TWISTER. The APTMS/PDMS sol-gel coating developed for SBSE was successfully applied for the determination of OPPs in grape and cucumber samples, and its performance was compared with commercial PDMS TWISTER. The recoveries of dicrotophos and malathion from cucumber and grape samples using APTMS/PDMS hybrid coating was 71% and 98%, respectively with RSD 3.1%-3.6%. The recoveries of malathion in cucumber and grape using PDMS-coated TWISTER was 91% and 62% respectively, with acceptable RSD 7.46%. SBSE using APTMS/PDMS hybrid coating showed better selectivity for the polar dicrotophos compared to commercial PDMS-coated TWISTER, which failed to extract the polar dicrotophos.
format	Thesis
qualification_level	Master's degree
author	Hasnan, Zafran
author_facet	Hasnan, Zafran
author_sort	Hasnan, Zafran
title	Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
title_short	Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
title_full	Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
title_fullStr	Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
title_full_unstemmed	Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
title_sort	sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2012
url	http://eprints.utm.my/id/eprint/28397/5/ZafranHasnanMFS2012.pdf
_version_	1747815643969748992

Sol-gel organic-inorganic hybrid polydimethysiloxane-3- aminopropyltrimethoxysilane as sorbent for stir bar sorpitive extraction of organophosphorus pesticides

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