scholarly journals Synthesis of Diazepam-Imprinted Polymers with Two Functional Monomers in Chloroform Using a Bulk Polymerization Method

2020 ◽  
Vol 2020 ◽  
pp. 1-8 ◽  
Author(s):  
Aliya Nur Hasanah ◽  
Dang Soni ◽  
Rimadani Pratiwi ◽  
Driyanti Rahayu ◽  
Sandra Megantara ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Methyl Methacrylate ◽  
Solid Phase ◽  
Bulk Polymerization ◽  
Phase Extraction ◽  
Serum Samples ◽  
Molecularly Imprinted ◽  
Functional Monomers ◽  
Other Substances ◽  
Polymerization Method

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.

scholarly journals Solid-phase extraction of selected acidic pharmaceuticals from wastewater using a molecularly imprinted polymer

2017 ◽  
Author(s):  
◽  
Silindile Senamile Zunngu
Keyword(s):  
Binding Energy ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Deionized Water ◽  
Phase Extraction ◽  
Functional Monomer ◽  
Imprinted Polymer ◽  
Molecularly Imprinted ◽  
Functional Monomers ◽  
Cross Linker

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.

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
Keyword(s):  
Solid Phase Extraction ◽  
Methacrylic Acid ◽  
Solid Phase ◽  
Bulk Polymerization ◽  
Degree Of Polymerization ◽  
Precipitation Polymerization ◽  
Therapeutic Effects ◽  
Phase Extraction ◽  
Functional Monomer ◽  
Polymerization Method

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.

scholarly journals Synergetic Effect of Dual Functional Monomers in Molecularly Imprinted Polymer Preparation for Selective Solid Phase Extraction of Ciprofloxacin

Polymers ◽  
2021 ◽  
Vol 13 (16) ◽  
pp. 2788
Author(s):  
Ut Dong Thach ◽  
Hong Hanh Nguyen Thi ◽  
Tuan Dung Pham ◽  
Hong Dao Mai ◽  
Tran-Thi Nhu-Trang
Keyword(s):  
Solid Phase Extraction ◽  
Molecularly Imprinted Polymer ◽  
Solid Phase ◽  
Template Molecule ◽  
Phase Extraction ◽  
Imprinted Polymer ◽  
Molecularly Imprinted ◽  
Functional Monomers ◽  
Imprinted Polymers ◽  
Dual Functional

Background: Ciprofloxacin (CIP), an important broad-spectrum fluoroquinolone antibiotic, was often used as a template molecule for the preparation of imprinted materials. In this study, methacrylic acid and 2-vinylpyridine were employed for the first time as dual functional monomers for synthesizing ciprofloxacin imprinted polymers. Methods: The chemical and physicochemical properties of synthesized polymers were characterized using Fourier transform-infrared spectroscopy, thermogravimetric analysis-differential scanning calorimetry, scanning electron microscopy, and nitrogen adsorption-desorption isotherm. The adsorption properties of ciprofloxacin onto synthesized polymers were determined by batch experiments. The extraction performances were studied using the solid phase extraction and HPCL-UV method. Results: The molecularly imprinted polymer synthesized with dual functional monomers showed a higher adsorption capacity and selectivity toward the template molecule. The adsorbed amounts of ciprofloxacin onto the imprinted and non-imprinted polymer were 2.40 and 1.45 mg g−1, respectively. Furthermore, the imprinted polymers were employed as a selective adsorbent for the solid phase extraction of ciprofloxacin in aqueous solutions with the recovery of 105% and relative standard deviation of 7.9%. This work provides an alternative approach for designing a new adsorbent with high adsorption capacity and good extraction performance for highly polar template molecules.

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
Keyword(s):  
Methyl Methacrylate ◽  
Solid Phase ◽  
Bulk Polymerization ◽  
Drug Analysis ◽  
Precipitation Polymerization ◽  
Functional Monomer ◽  
Serum Samples ◽  
Imprinted Polymers ◽  
Polymerization Method ◽  
Spiked Serum

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.

Synthesis and application of a molecularly imprinted polymer in selective solid-phase extraction of efavirenz from water

2019 ◽  
Vol 79 (2) ◽  
pp. 356-365 ◽  
Author(s):  
Sinothando P. Mtolo ◽  
Precious N. Mahlambi ◽  
Lawrence M. Madikizela
Keyword(s):  
Surface Water ◽  
Solid Phase Extraction ◽  
Molecularly Imprinted Polymer ◽  
Solid Phase ◽  
Bulk Polymerization ◽  
Antiretroviral Drugs ◽  
Array Detector ◽  
Phase Extraction ◽  
Imprinted Polymer ◽  
Molecularly Imprinted

Abstract Efavirenz is one of the antiretroviral drugs widely used to treat the human immunodeficiency virus. Antiretroviral drugs have been found to be present in surface water and wastewater. Due to complexity of environmental samples, solid-phase extraction (SPE) is used for isolation and pre-concentration of antiretroviral drugs prior to their chromatographic analysis. However, the commercially available SPE sorbents lack selectivity, which tends to prolong the analysis time. Therefore, in this study a molecularly imprinted polymer was synthesized for the specific recognition of efavirenz and then applied as the SPE sorbent for its extraction from wastewater and surface water samples. The imprinted and non-imprinted polymers were synthesized using a bulk polymerization technique where efavirenz was used as the template, 2-vinylpyridine as functional monomer, 1,1′-azobis-(cyclohexanecarbonitrile) as initiator, ethylene glycol dimethacrylate as cross-linker and toluene:acetonitrile (9:1, v/v) as the porogenic solvent mixture. The characterization was performed using Fourier transform infrared spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller, elemental analysis, and thermogravimetric analysis techniques. Results showed better selectivity of molecularly imprinted polymer to efavirenz than did non-imprinted polymer. The analysis was performed using high performance liquid chromatography equipped with a photo-diode array detector. The analytical method gave a detection limit of 0.41 μg/L and the analyte recovery of 81% in wastewater. The concentrations found in wastewater ranged from 2.79 to 120.7 μg/L, while in surface water they were between 0.975 and 2.88 μg/L. Therefore, the results of this study show a strong need for a detailed screening of efavirenz in major water utilities in the country.

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