Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography

A simple and rapid method has been developed for the determination of organophosphorus (OP), organochlorine (OC), and pyrethriod (PY) pesticides in vegetables using solid-phase extraction (SPE) cleanup. The results obtained were compared with the established routine method without cleanup for OP pes...

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Main Author: Cha, Lian Kuet.
Format: Thesis
Language:English
Published: 2003
Subjects:
Online Access:http://ir.unimas.my/id/eprint/24790/1/Chai%20Lian%20Kuet%20ft.pdf
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spelling my-unimas-ir.247902023-05-10T07:39:00Z Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography 2003 Cha, Lian Kuet. Q Science (General) QD Chemistry A simple and rapid method has been developed for the determination of organophosphorus (OP), organochlorine (OC), and pyrethriod (PY) pesticides in vegetables using solid-phase extraction (SPE) cleanup. The results obtained were compared with the established routine method without cleanup for OP pesticides and silica gel cleanup for OC and PYpesticides. Residues were extracted with acetone and methylene chloride lJfxtracts were cleanup up by SPE mixed-mode column using quaternary amine and aminopropyl (SAXINH2) or octadecyl (CI8) sorbents. The pesticides were determined by gas chromatography with flame photometric detector for OP pesticides and micro-electron capture detector (u-ECD) for OC and PY pesticides. The results from the SAXINH2study showed that the recoveries obtained for the eleven OP pesticides tested except for the polar one such as methamidophos and dimethoate (depending on the matrix) were within the acceptable range of 70 % to 120 %. This method offers a cleaner extract than the routine method which do not requires cleanup. The extract obtained can be injected directly into the ECD for the OC and PY determination. Recoveries obtained for the six OC pesticides using the same method were comparable with the silica gel method. For the five PYpesticides tested, the recoveries obtained were also corresponding to the silica gel method. For the CI8 cleanup method, the recoveries obtainedfor eleven OP pesticides tested except methamidophos were within the acceptable range. However, the recoveries obtainedfor the nine OC pesticides using the CI8 method were lower than those obtained from silica gel method. For the five PYpesticides tested, the recoveries obtained using this method were comparable to the silica gel method. In spite of the limited range of this study, it can be predicted that the SPE CI8 and SAXINH2 cleanup methods can be extrapolated to a wider range of other OP, OC and PY pesticides. These methods can also be used for other fruits and vegetables. The benefits of the SPE method compared to the routine method were the used of organic solvents is reduced, possibility of concentration of the samples, less sorbent used, no cross contamination, shorter analysis time and the technique is easy to automate. Universiti Malaysia Sarawak (UNIMAS) 2003 Thesis http://ir.unimas.my/id/eprint/24790/ http://ir.unimas.my/id/eprint/24790/1/Chai%20Lian%20Kuet%20ft.pdf text en validuser masters Universiti Malaysia Sarawak Faculty of Resource Science and Technology
institution Universiti Malaysia Sarawak
collection UNIMAS Institutional Repository
language English
topic Q Science (General)
QD Chemistry
spellingShingle Q Science (General)
QD Chemistry
Cha, Lian Kuet.
Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
description A simple and rapid method has been developed for the determination of organophosphorus (OP), organochlorine (OC), and pyrethriod (PY) pesticides in vegetables using solid-phase extraction (SPE) cleanup. The results obtained were compared with the established routine method without cleanup for OP pesticides and silica gel cleanup for OC and PYpesticides. Residues were extracted with acetone and methylene chloride lJfxtracts were cleanup up by SPE mixed-mode column using quaternary amine and aminopropyl (SAXINH2) or octadecyl (CI8) sorbents. The pesticides were determined by gas chromatography with flame photometric detector for OP pesticides and micro-electron capture detector (u-ECD) for OC and PY pesticides. The results from the SAXINH2study showed that the recoveries obtained for the eleven OP pesticides tested except for the polar one such as methamidophos and dimethoate (depending on the matrix) were within the acceptable range of 70 % to 120 %. This method offers a cleaner extract than the routine method which do not requires cleanup. The extract obtained can be injected directly into the ECD for the OC and PY determination. Recoveries obtained for the six OC pesticides using the same method were comparable with the silica gel method. For the five PYpesticides tested, the recoveries obtained were also corresponding to the silica gel method. For the CI8 cleanup method, the recoveries obtainedfor eleven OP pesticides tested except methamidophos were within the acceptable range. However, the recoveries obtainedfor the nine OC pesticides using the CI8 method were lower than those obtained from silica gel method. For the five PYpesticides tested, the recoveries obtained using this method were comparable to the silica gel method. In spite of the limited range of this study, it can be predicted that the SPE CI8 and SAXINH2 cleanup methods can be extrapolated to a wider range of other OP, OC and PY pesticides. These methods can also be used for other fruits and vegetables. The benefits of the SPE method compared to the routine method were the used of organic solvents is reduced, possibility of concentration of the samples, less sorbent used, no cross contamination, shorter analysis time and the technique is easy to automate.
format Thesis
qualification_level Master's degree
author Cha, Lian Kuet.
author_facet Cha, Lian Kuet.
author_sort Cha, Lian Kuet.
title Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
title_short Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
title_full Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
title_fullStr Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
title_full_unstemmed Simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
title_sort simultaneous determination of presticide residues in vegetables by solid-phase extraction cleanup and gas chromatography
granting_institution Universiti Malaysia Sarawak
granting_department Faculty of Resource Science and Technology
publishDate 2003
url http://ir.unimas.my/id/eprint/24790/1/Chai%20Lian%20Kuet%20ft.pdf
_version_ 1783728270249820160