Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar

In this study, a novel selective sorbent was prepared by immobilization of NBoc-Phenylalanine-NBoc-Histidine (BCPA) chiral selector with modified polydimethylsiloxane (PDMS) surface for the isolation of the (S)-isomer in cypermethrin (CPM) compound prior to its determination by gas chromatography-mi...

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Main Author:	Masdar, Non Daina
Format:	Thesis
Language:	English
Published:	2020
Subjects:	Theory of solution
Online Access:	https://ir.uitm.edu.my/id/eprint/59750/1/59750.pdf
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spelling	my-uitm-ir.597502022-05-17T08:16:24Z Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar 2020-12 Masdar, Non Daina Theory of solution In this study, a novel selective sorbent was prepared by immobilization of NBoc-Phenylalanine-NBoc-Histidine (BCPA) chiral selector with modified polydimethylsiloxane (PDMS) surface for the isolation of the (S)-isomer in cypermethrin (CPM) compound prior to its determination by gas chromatography-micro electron captured detector (GC-ECD). Characterization of the newly synthesized sorbent material was performed using attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), nuclear magnetic resonance (NMR), emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and Tensiometer (TM) to correlate sorbent characteristics with their performance. ATR-FTIR and NMR studies indicate strong hydrogen bonding interactions between polydimethylsiloxane and NBoc-Phenylalanine-NBoc-Histidine chiral selector (BCPA) immobilization. XPS indicates the elemental composition and chemical state of the chiral selector that exists within the immobilized structure. The applicability of the new sorbent for the isolation of (S)-isomer from alpha cypermethrin (ACPM) standard compound was examined by direct solid-liquid interface adsorption method followed by GC-ECD analysis. Response surface methodology (RSM) was applied to assist the optimization of both adsorption and GC methods. The enantioseparation of the CPM compound was performed on a CycloSil B capillary column. The calibration curve was linear in the range of 0.020 -1.200 gmL-1 with correlation coefficient (R2) of 0.9612. Limit of detection and limit of quantification were 0.467 and 1.41 gmL-1, respectively, and acceptable recoveries were achieved in the range of 66.44 to 118.82 %. Results show that the incorporation of NBoc-Phenylalanine-NBoc-Histidine chiral selector with modified PDMS surface polymer had provided an enantiomer discriminating capability to the sorbent. It indicates that NBoc-Phenylalanine-NBoc-Histidine chiral selector had specifically exhibited enantio-selectivity for (S)-isomer. An analytical Eco-Scale was then measured as an approach to evaluate the greenness of this analytical methodology. The Eco-Scale score of 77 results from the minimal reagent/solvents used in this analysis proves that this straightforward isolation method can be considered as an excellent green analysis that is highly selective towards (S)-isomer. 2020-12 Thesis https://ir.uitm.edu.my/id/eprint/59750/ https://ir.uitm.edu.my/id/eprint/59750/1/59750.pdf text en public phd doctoral Universiti Teknologi MARA Faculty of Applied Sciences Saim, Norashikin (Professor Dr.) Tajuddin, Ruziyati (Dr.) Md Jani, Abd Mutalib (Associate Professor Dr.) Mohd Ali, Muhamad Tajuddin (Dr.)
institution	Universiti Teknologi MARA
collection	UiTM Institutional Repository
language	English
advisor	Saim, Norashikin (Professor Dr.) Tajuddin, Ruziyati (Dr.) Md Jani, Abd Mutalib (Associate Professor Dr.) Mohd Ali, Muhamad Tajuddin (Dr.)
topic	Theory of solution
spellingShingle	Theory of solution Masdar, Non Daina Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
description	In this study, a novel selective sorbent was prepared by immobilization of NBoc-Phenylalanine-NBoc-Histidine (BCPA) chiral selector with modified polydimethylsiloxane (PDMS) surface for the isolation of the (S)-isomer in cypermethrin (CPM) compound prior to its determination by gas chromatography-micro electron captured detector (GC-ECD). Characterization of the newly synthesized sorbent material was performed using attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), nuclear magnetic resonance (NMR), emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and Tensiometer (TM) to correlate sorbent characteristics with their performance. ATR-FTIR and NMR studies indicate strong hydrogen bonding interactions between polydimethylsiloxane and NBoc-Phenylalanine-NBoc-Histidine chiral selector (BCPA) immobilization. XPS indicates the elemental composition and chemical state of the chiral selector that exists within the immobilized structure. The applicability of the new sorbent for the isolation of (S)-isomer from alpha cypermethrin (ACPM) standard compound was examined by direct solid-liquid interface adsorption method followed by GC-ECD analysis. Response surface methodology (RSM) was applied to assist the optimization of both adsorption and GC methods. The enantioseparation of the CPM compound was performed on a CycloSil B capillary column. The calibration curve was linear in the range of 0.020 -1.200 gmL-1 with correlation coefficient (R2) of 0.9612. Limit of detection and limit of quantification were 0.467 and 1.41 gmL-1, respectively, and acceptable recoveries were achieved in the range of 66.44 to 118.82 %. Results show that the incorporation of NBoc-Phenylalanine-NBoc-Histidine chiral selector with modified PDMS surface polymer had provided an enantiomer discriminating capability to the sorbent. It indicates that NBoc-Phenylalanine-NBoc-Histidine chiral selector had specifically exhibited enantio-selectivity for (S)-isomer. An analytical Eco-Scale was then measured as an approach to evaluate the greenness of this analytical methodology. The Eco-Scale score of 77 results from the minimal reagent/solvents used in this analysis proves that this straightforward isolation method can be considered as an excellent green analysis that is highly selective towards (S)-isomer.
format	Thesis
qualification_name	Doctor of Philosophy (PhD.)
qualification_level	Doctorate
author	Masdar, Non Daina
author_facet	Masdar, Non Daina
author_sort	Masdar, Non Daina
title	Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
title_short	Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
title_full	Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
title_fullStr	Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
title_full_unstemmed	Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar
title_sort	modified polydimethylsiloxane surface as selective sorbent for the isolation of (s)-isomer in cypermethrin / non daina masdar
granting_institution	Universiti Teknologi MARA
granting_department	Faculty of Applied Sciences
publishDate	2020
url	https://ir.uitm.edu.my/id/eprint/59750/1/59750.pdf
_version_	1783735052207652864

Modified polydimethylsiloxane surface as selective sorbent for the isolation of (S)-isomer in cypermethrin / Non Daina Masdar

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