scholarly journals Synthesis of Atenolol-Imprinted Polymers with Methyl Methacrylate as Functional Monomer in Propanol Using Bulk and Precipitation Polymerization Method

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Aliya Nur Hasanah ◽  
Traju Ningtias Dwi Utari ◽  
Rimadani Pratiwi

Atenolol is one of the beta-1 blocker drugs that is misused by athletes to increase their performance during competition. Therefore, it is important to analyze atenolol levels in blood selectively. The preparation method that can be used in separating atenolol in sample is molecular imprinting solid-phase extraction (MI-SPE) because it has good selectivity and sensitivity. This study aims to examine the characteristics and analytical performance of imprinted polymers synthesized from functional monomer methyl methacrylate. The stages of this study include the determination of association constants, synthesis of sorbent MI-SPE atenolol using the bulk polymerization method, and precipitation with atenolol as the template, methyl methacrylate as the functional monomer, and propanol as the porogen. The template was extracted from a polymer, and then, the adsorption ability, capacity, and selectivity of MI-SPE and finally the application of the best MI-SPE to spiked serum samples were determined. MI-SPE was also characterized by using Fourier-transform instrument infrared (FTIR) and scanning electron microscope (SEM). The result of characterization with FTIR and SEM showed that MIP made by the precipitation polymerization method was completely polymerized, more porous, and produced smaller particle size with an average value of 0.274 μm. It had better analytic performances than MIP made by bulk polymerization, with affinity value 0.3607 mg/g and homogeneity value 1.3246, and good selectivity toward atenolol with imprinting factor value 22.519. Application of MI-SPE to spiked serum samples has an excellent recovery percentage of 95.46% over 0% for the nonimprinting one. Based on the result of study, MIP made by precipitation polymerization could be used to extract atenolol on serum samples toward drug analysis.

2020 ◽  
Vol 10 (3) ◽  
pp. 277-288
Author(s):  
Aliya Nur Hasanah ◽  
Diane Fauzi ◽  
Beska Zausha Witka ◽  
Driyanti Rahayu ◽  
Rimadani Pratiwi

Ethylmorphine is an opioid that has therapeutic effects as narcotic analgesic and antitussive, which has low levels and can be misused. Hence, it is crucial to monitor by analyze the levels of ethylmorphine in blood selectively. The preparation method that can be used to extract ethylmorphine from the sample is using molecular imprinting solid-phase extraction (MI-SPE) due to its sensitivity and selectivity. This study aims to compare the result of synthesis using two different polymerization methods, and also to examine the analytical performance and characteristics of imprinted polymers from two distinct functional monomers: methacrylic acid (MAA) and acrylamide (AM). The stages of this study include the determination of association constants, synthesis of polymer MI-SPE ethylmorphine using bulk and precipitation polymerization method, extracted template from the polymer, and determined the adsorption ability, capacity, and selectivity of the polymer. MI-SPE that has been made then characterized by using Fourier-Transform Infrared (FTIR) and Scanning Electron Microscope (SEM). The results showed that MIP with acrylamide (MIP-AM) as functional monomer and made by precipitation polymerization had better analytic performances than MIP that made by bulk polymerization, with affinity value 0.072 mg/g and homogeneity value -0.77. It is also selective toward ethylmorphine with imprinting factor value 27.43. In addition, the result of characterization using FTIR and SEM showed that MIP-AM 2, MIP-MAA 1, and MIP-MAA 2 might have a low degree of polymerization due to the presence of vinyl peaks, besides MIP-AM 2 and MIP-MAA 2 had smaller particle size than the NIP with an average value of 0,31 ± 0,21 mm and 0.28 ± 0.05 mm. Based on the result of this study, MIP-AM made by precipitation polymerization could be used to extract ethylmorphine on solid-phase extraction.


2020 ◽  
Vol 2020 ◽  
pp. 1-8 ◽  
Author(s):  
Aliya Nur Hasanah ◽  
Dang Soni ◽  
Rimadani Pratiwi ◽  
Driyanti Rahayu ◽  
Sandra Megantara ◽  
...  

Diazepam is a benzodiazepine that has the potency to be misused because it is effective, easily obtained, and inexpensive. The misuse of diazepam is to replace illegal drugs and be a sedative. Separation of diazepam is needed to detect possible drug abuse and to monitor drug levels in blood to ensure the effectiveness of the drug. This study was conducted to obtain a molecularly imprinted solid-phase extraction (MI-SPE) sorbent to separate diazepam from serum samples. This work started at the synthesis stage with the bulk polymerization method, using methyl methacrylate and acrylamide as functional monomers, diazepam as a template, and ethylene glycol dimethacrylate as a crosslinker. The polymer obtained was identified by its adsorption capacity and packaged into a solid-phase extraction (SPE) cartridge, and the extraction conditions were optimized. The optimization results were then used to extract diazepam from the serum sample. The test results showed that the adsorption ability of the molecularly imprinted polymer (MIP) with the functional monomer, methyl methacrylate, was 63.98 ± 0.1%, which is higher than that of the acrylamide MIP monomer, with a value of 43.27 ± 0.1%. The MIP sorbent of methyl methacrylate was applied to the SPE with 200 mg of polymer in a 3 mL cartridge. Diazepam added to serum samples were then passed through the MIP-SPE producing a percent recovery value of 95.31 ± 1.1% for MIP and 60.83 ± 0.3% for nonimprinted polymer (NIP). The results showed that the MI-SPE sorbent made from the monomer methyl methacrylate gave higher extraction recovery results than acrylamide, and it could be used for extracting diazepam from serum samples with or without other substances.


2011 ◽  
Vol 399-401 ◽  
pp. 713-717 ◽  
Author(s):  
Xu Hong Jiang ◽  
Zhan Mei Liu

Uniformly-sized, molecularly imprinted polymers (MIPs) for (D)-naproxen have been prepared by a precipitation polymerization method using methacrylic acid (MAA) as a functional monomer and divinylbenzene (DVB) as a cross-linker in acetonitrile or a mixture of toluene and acetonitrile(1:3). The (D)-naproxen-imprinted MAA-co-DVB polymers were monodispersed microspheres with size in the range of 1.5 to 3.6µm. Enantioseparation of naproxen was attained using the (D)-naproxen-imprinted MAA-co-DVB polymer microspheres. When Ethylene glycol dimethacrylate(EGDMA) was used as a cross-linker, the MAA-co -EGDMA polymers were sub-microspheres with the average size of 350nm and showed very low affinity for the template (D)-naproxen . The (D)-naproxen-imprinted MAA-co-DVB polymer microspheres prepared in the mixture of toluene showed the highest molecular recognition ability and with the biggest size of 3.6µm.


2019 ◽  
Vol 19 (1) ◽  
pp. 219
Author(s):  
Hemavathi Krishnan ◽  
A.K.M. Shafiqul Islam ◽  
Zainab Hamzah ◽  
Pubalan Nadaraja ◽  
Mohd Noor Ahmad

The use of molecularly imprinted polymers for Solid phase micro-extraction (SPME) of bioactive compounds are getting popularity. The interest on efficient extraction process of andrographolide from the plant is increasing due to their vast therapeutic applications. In this study, andrographolide imprinted MIP was prepared by precipitation polymerization method using the non-covalent technique to use as sorbent materials for solid phase extraction of the bioactive compound. HyperChem 8.0.10 software was used to investigate and optimize the template and functional monomer ratio in the pre-polymerization system to synthesize the imprinted polymers. Molecular modeling gives information about molecular interactions and the Gibbs free energies of the pre-polymerization complex. Based on the computational study, andrographolide, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) were used as the template, functional monomer, and cross-linker, respectively at the 1:3:20 ratios. The MIPs were characterized by kinetic study and imprinting factor. The binding parameters for the recognition of andrographolide were studied using Langmuir, Freundlich and Langmuir-Freundlich adsorption isotherm models. Andrographolide MIP contains the maximum number of binding sites with the adsorption capacity of 149.59 μg/g. The SPME experimental data best fit with Langmuir-Freundlich isotherm model with the R2 value of 0.997. This research shows that the MIPs prepared by precipitation polymerization gives a good extraction capability using SPME method.


2019 ◽  
Vol 11 (1) ◽  
pp. 136
Author(s):  
Aliya Nur Hasanah ◽  
Asri Budi Yulianti ◽  
Driyanti Rahayu

Objective: This study was aimed to determine analytical performance and physical character of MI-SPE (Molecular Imprinted Solid Phase Extraction) atenolol using itaconic acid as the functional monomer and to implement the material for the extraction of atenolol in blood serum.Methods: This experiment was performed by determining association constants between monomer-template with UV-Vis spectrophotometer, the synthesis of MI-SPE atenolol using bulk polymerization method, template extraction, evaluation of the adsorption ability and capacity of sorbent, evaluation of sorbent selectivity, and determining their physical character using Fourier Transform Infrared (FTIR) and Scanning Electron Microscope (SEM). In the end, the sorbent then was implemented to extract atenolol in blood serum.Results: Analytical performance showed that MI-SPE sorbent has Imprinting Factor (IF) 10.632 which is the largest number compared to IF when using another beta blocker compound. Physical characterization obtained by MI-SPE using Scanning Electron Microscope (SEM) method showed that MI-SPE morphology has homogeneous pore and number of cavities than its blank. MI-SPE has recovery percentage 92.22 % atenolol when it applied to blood serum spiked with atenolol standard.Conclusion: MI-SPE sorbent made from the itaconic acid monomer in methanol porogen potential to be used for the extraction of atenolol from the blood sample by selectively bind to atenolol.


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