Synthesis Of Molecularly Imprinted Polymer For Selective Solid-Phase Extraction Of Salbutamol From Urine Samples
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Date
2011-11
Authors
Lee, Wei Inn
Journal Title
Journal ISSN
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Publisher
Universiti Sains Malaysia
Abstract
High selective molecularly imprinted polymers were synthesized to extracted salbutamol from human urine samples using structurally analogue template molecules. Molecularly imprinted polymers (MIPs) were prepared by using bamethane (BIP) and methylated salbutamol (CIP), two structural analogue of the targeted analyte, salbutamol as template. Free radical polymerization was conducted in a non-covalent approach using methacrylic acid (MAA) as functional monomer and ethylene glycol methacrylate (EGDMA) as cross-linking agent. The polymerization process was initiated by 2,2‟-azobisdimethyl valeronitrile and conducted at 50 ºC for 24 hours. Molar ratio of template molecule: functional monomer: cross-linking agent was fixed at 1:4:20. A macroporous monolith polymer was formed, grinding and sieving was required to obtain the particles with size between 40 and 75 μm. The particles obtained were subjected to Soxhlet extraction for the removal of template in order to create recognition sites. An equivalent non-imprinted polymer was synthesized simultaneously using the same procedure but in the absence of template molecule. In selectivity experiments, significant differences in the elution profile between the polymers were observed. With the imprinted polymers, specific binding toward targeted analyte occurred. However, with the blank polymer, only weak and non-specific interaction occurred. Cross-specificity studies showed that the MIPs had molecular recognition properties towards other compounds that are structurally related to salbutamol, such as clenbuterol, fenoterol, isoxsuprine, metoprolol, ractopamine and terbutaline. IR and 1H NMR analysis were done to study the interaction between analytes and monomer. Hydrogen bonding was proven to exist in between analytes and monomer. The MIPs were used in the solid phase extraction of spiked human urine samples prior to GC-MS.
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Keywords
Synthesis of molecularly imprinted polymer , solid-phase extraction of salbutamol from urine samples