scholarly journals Molecular Imprinted Polymer for Ethylmorphine with Methacrylic Acid and Acrylamide as Functional Monomer in Butanol Using Two Polymerization Method

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.

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 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.


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.


2017 ◽  
Author(s):  
◽  
Silindile Senamile Zunngu

In this study, molecular modeling was used to investigate the intermolecular interactions between the functional monomer and ketoprofen which is an acidic pharmaceutical that possesses anti-inflammatory and analgesic activities. Ketoprofen is widely employed in medical care for treating musculoskeletal injury. This led to rational design of a molecularly imprinted polymer (MIP) that is selective to ketoprofen. Density functional theory (DFT) at B3LYP/6-31 level was used to investigate the intermolecular interaction between functional monomers and ketoprofen. Binding energy, ΔE, was used as an indication of the strength of the interaction that occurs between functional monomers and ketoprofen. 2-vinylpyridine (2-VP) as one of the functional monomers gave the lowest binding energy when compared to all the functional monomers investigated. Monomer-template interactions were further experimentally investigated using spectroscopic techniques such as Ultraviolet-visible and Fourier transform infrared (FTIR). A selective MIP for ketoprofen was synthesized using 2-vinylpyridine, ethylene glycol dimethacrylate, 1,1’-azobis(cyclohexanecarbonitrile), toluene/acetonitrile (9:1, v/v), and ketoprofen as a functional monomer, cross-linker, initiator, porogenic mixture, and template, respectively. The polymerization was performed at 60 °C for 16 h, and thereafter the temperature was increased to 80 °C for 24 h to achieve a solid monolith polymer. The non-imprinted polymer (NIP) was synthesized in a similar manner with the omission of ketoprofen. Characterization with thermogravimetric analysis (TGA) and powder X-ray diffraction (XRD) showed that the synthesized polymers were thermally stable and amorphous. Morphology of the particles were clearly visible, with MIP showing rough and irregular surface compared to NIP on the scanning electron microscopy (SEM). The characterization of the prominent functional groups on both MIP and NIP were performed using FTIR and nuclear magnetic resonance (NMR). The existence of hydroxyl was observed in the MIP; this was due to the presence of ketoprofen in the cavity. Prominent carbonyl group was an indication of the cross-linker present in both polymers. The synthesized MIP was applied as a selective sorbent in the solid-phase extraction of ketoprofen from the water. The extracted ketoprofen was monitored by high performance liquid chromatography (HPLC) coupled with UV/Vis detector. Several parameters were investigated for maximum recovery of ketoprofen from the spiked deionized water. The optimum method involved the conditioning of 14 mg MIP sorbent with 5 mL of methanol followed by equilibrating with 5 mL of deionized water adjusted to pH 2.5. Thereafter, 50 mL sample (pH 5) was loaded into the cartridge containing MIP sorbent followed by washing and eluting with 1% TEA/H2O and 100% methanol, respectively. Eluted compounds were quantified with HPLC. MIP was more selective to ketoprofen in the presence of other structural related competitors. The analytical method gave detection limits of 0.23, 0.17, and 0.09 mg L-1 in wastewater influent, effluent, and deionized water, respectively. The recovery for the wastewater influent and effluent spiked with 5 µg L-1 of ketoprofen was 68%, whereas 114% was obtained for deionized water. The concentrations of ketoprofen in the influent and effluent samples were in the ranges of 22.5 - 34.0 and 1.14 - 5.33 mg.L-1, respectively. The relative standard deviation (RSD) given as ± values indicates that the developed analytical method for the analysis of ketoprofen in wastewater was rapid, affordable, accurate, precise, sensitive, and selective.


2020 ◽  
Vol 12 (47) ◽  
pp. 5729-5736
Author(s):  
Simone Cavalera ◽  
Fabio Di Nardo ◽  
Giulia Spano ◽  
Laura Anfossi ◽  
Panagiotis Manesiotis ◽  
...  

A selective molecularly imprinted polymer prepared with a squaramide-based functional monomer was used for the solid phase extraction of roxarsone from surface waters.


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