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![Schematic illustration of theophylline extraction from the as-prepared polymer and its guest-binding [6]](publication/308539226/figure/fig2/AS:410604910202881@1474907247984/Schematic-illustration-of-theophylline-extraction-from-the-as-prepared-polymer-and-its.png)
Schematic illustration of theophylline extraction from the as-prepared polymer and its guest-binding [6]
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A molecularly imprinted polymer (MIP) based on methacrylic acid (MAA) monomer and theophylline template has been synthesized using a modified bulk polymerization method. Theophylline was employed as a template and it formed a complex with MAA through hydrogen bonding. Self-assembly of template-monomer was followed by cross-linking process using eth...
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... Metode ini dipilih, karena waktu yang dibutuhkan dalam prosesnya lebih singkat dibandingkan metode sintesis lain yang pada umumnya telah dilakukan [5,6]. Metode sederhana ini telah diaplikasikan dalam banyak zat aktif, diantaranya melamin dan kafein, dan theophylline [6,7,8,9]. Dalam artikel ini dilaporkan bagaimana metode cooling-heating telah berhasil diterapkan untuk ion Fe (III). ...
Polimer Fe(III) berbasis Ion Imprinted Polymers atau yang disebut IIPs-Fe (III) telah berhasil disintesis menggunakan metode cooling-heating dengan asam metakrilat (MAA) sebagai monomer fungsi, etilen glikoldimetakrilat (EDGMA) sebagai pengikat silang, benzoil peroksida (BPO) sebagai inisiator, dan acetonitril sebagai pelarut. NIP (Non Imprinted Polymer) juga disintesis tanpa menggunakan zat aktif Fe(III) yang berfungsi sebagai polimer pembanding. Polimer Fe(III) yang dihasilkan selanjutnya digerus dan diekstraksi dengan menggunakan etanol (8,5 mL), air deionisasi (15 mL), dan HCl (8 mL; 1 M) untuk memisahkan ion Fe (III) dari polimer. Setelah diekstraksi kemudian hasilnya dikarakterisasi menggunakan FTIR, XRD dan SEM. Hasil FTIR menunjukkan adanya gugus fungsi khas pada setiap ikatan atom yang menjadi penyusun pada polimer IIPs-Fe(III). Berdasarkan hasil FTIR, terjadi perubahan % transmitansi pada polimer sebelum dan setelah ekstraksi, yaitu untuk gugus C=O nilai % transmitansi berubah dari 75% menjadi 82,5%, gugus C-H dari 94% menjadi 95%, gugus C-O dari 74% menjadi 75%, dan gugus C=N dari 92,5% menjadi 95%. Hal ini menunjukkan bahwa ion Fe(III) telah berkurang dari IIPs-Fe(III) akibat proses ektraksi. Hasil XRD menunjukkan bahwa nilai FWHM sedikit turun dari 1,911 nm menjadi 1,910 nm. Hal ini menunjukkan tidak terjadi perubahan yang signifikan pada ukuran kristalitnya. Sedangkan dari analisis SEM diperoleh informasi bahwa jumlah rongga yang tercipta pada IIPs-Fe (III) untuk ukuran <100nm sebanyak 237 rongga.
... For example, previous ca eine MIP polymerization processes takes 16 hours (Farrington et al., 2006) , 24 hours (Hidayat and Sunarto, 2017) , and 48 hours (Cormack and Mehamod, 2013) to complete using nitrogen ow and immersing the polymer into a water bath. However, this duration can be overcome using the cooling-heating method in the polymerization process, which was tested in several active substances without reducing the characteristics of the resulting polymer (Royani and Abdullah, 2014;Nurhayati et al., 2016;Koriyanti et al., 2020). ...
The cooling-heating method was used to successfully synthesize molecularly imprinted polymers on caffeine. Caffeine was used as a template and mixed with chloroform solvent, methacrylic acid as a monomer, ethylene glycol dimethacrylate as a cross-linker, and benzoyl peroxide as an initiator. The solution was stirred for 15 minutes and placed in a vial. Then it was placed in a cooler with a temperature of -5○C for 60 minutes and then inserted into an oven with an increasing temperature at 75○C, 80○C, and 85○C for 3, 2 and 1 hour, respectively. Furthermore, the repeated washing process resulted in solid polymer, which was subjected to template leaching to produce polymers with specific cavities called molecularly imprinted polymers (MIP). The resulting caffeine polymer and MIP were tested using SEM, FTIR, and XRD methods. In addition, the SEM image analysis data showed 388 cavities in the polymer after template leaching, compared to the 121 cavities in the unwashed polymer. This result was supported by the FTIR spectrum analysis which showed that caffeine MIP has a higher transmittance value than the polymer. Therefore, the caffeine concentration was significantly reduced after the leaching process. The XRD spectra showed that caffeine MIP had a smaller halfmaximum diffraction peak width (FWHM) compared to the polymer. Also, the low FWHM value depicted a larger crystalline size in the caffeine MIP compared to the polymer.
... The polymer from the precipitation method was then separated using centrifugation and rinsed with 20 mL of methanol and water mixture, and dried again in the oven for 18 h at 70°C. The same procedure was carried out for making NIP but without the addition of the DZP template [15]. ...
... The ratio between monomers and templates contributes to the observations of the interaction between the two components. The ratio between the itaconic acid and DZP used was arranged in such a manner through optimisation stages and according to the ideal ratio (ro) ≥100 [14,15]. ...
... Synthesis of MIP and NIP following the free radical polymerisation reaction was initiated by the thermal decomposition of BPO as an initiator after the mixture was put into the oven [15]. BPO is active in the form of free radicals and initiates polymerisation by giving free electron pairs to carbon monomer double bonds that will then form carbon radicals. ...
Diazepam (DZP) is a benzodiazepine drug used as an anti-drug and sedative. It is often misused to induce or create euphoria in combination with other drugs (high or fly sensation) or administered alone. So far, screening for DZP abuse with sensitive analytical methods is needed, as its small concentrations make it difficult to detect. Increased sensitivity of the analytical method can be obtained by using a preparation method that selectively separates the analyte from the sample matrix. Molecularly imprinted polymer (MIP) is one of the preparation solutions with good selectivity, specificity, and sensitivity. MIP was made from DZP as a template, itaconic acid, and ethylene glycol dimethacrylate in a composition of 1:4:20. MIP was made by precipitation polymerisation to obtain microsphere polymer type. MIP had a binding capacity value of 0.0557 mg/g and followed the Freundlich isotherm. Application of the microsphere MIP on spiked blood serum resulted in a recovery of 105.63 ± 1.0% for MIP compared to 21.28 ± 0.4% for non-imprinted polymer, with the imprinting factor value reaching 4.96. Hence, MIP DZP with itaconic acid as a functional monomer and propanol as a porogen, fabricated by the precipitation polymerisation method, is a promising sorbent for DZP extraction in biological fluids.
... cm -1 . Stretching band due to N-H of imidazole ring from THP is absent or shifted at 2915.12cm -1 in both the ICs [36]. The C-H stretching due to methyl group are shifted to 2915.12cm -1 in both ICs and carbonyl C=O stretching shifted to 1620 cm -1 in α-CYD+THP & 1614.19cm ...
Steady host–guest inclusion complexes have been produced with medicinally important guest molecule theophylline within aqueous α-Cyclodextrin and HP-β-Cyclodextrin. α-and HP-β-Cyclodextrins have been established with favorable structural features for inclusion with Theophylline which include diversified applications in modern science such as controlled delivery in the field of pharmaceuticals, food processing, pesticides, foodstuffs etc. Theophylline is one of the most widely accepted drugs for the treatment of asthma and chronic obstructive pulmonary disease (COPD) worldwide, even if it has been used clinically for many years. With both α and HP-β-Cyclodextrins it is found that 1:1 hosts-guest inclusion complexes are formed with the guest molecule theophylline. The construction and quality of the inclusion complexes have been characterized by using conductivity measurement, surface tension study, and Job’s method. The inclusion phenomenon has been confirmed by FTIR spectroscopy, proton NMR study. Association constants and thermodynamic parameters have been evaluated for the created inclusion complexes by ultraviolet spectroscopy.
... The binding constant was estimated using the Benesi-Hildebrand equation. 11 Synthesis of Molecularly Imprinted Polymer Bulk polymerization was carried out using atenolol as a template (0.2663 g), MMA as a functional monomer (400 µL), EGDMA as the crosslinker (3.77 mL), and BPO as the initiator (750 mg). All of these were dissolved in 10 mL of porogen solvent in a tube. ...
... Non-imprinted polymers (NIPs) were prepped using the same method for the MIPs without the addition of the template in the polymerization. 11,12 Precipitation polymerization was carried out using atenolol as a template (0.2663 g) and it was dissolved in butanol (50 mL) in the bottle. The mixture then was sonicated for five minutes. ...
... Telah dilaporkan dalam tulisan Royani dkk pada tahun 2014, bagaimana cara menggunakan metode cooling-heating dalam pembuatan MIP atrazin. Selain MIP atrazin, metode cooling-heating juga telah diterapkan dalam pembuatan MIP glukosa dan MIP theophylline [16,17]. Metode cooling-heating adalah metode yang menggunakan proses pendinginan dan pemanasan pada proses polimerisasi. ...
... Metode cooling-heating adalah metode yang menggunakan proses pendinginan dan pemanasan pada proses polimerisasi. Waktu yang dihasilkan dari metode cooling-heating lebih efisien jika dibandingkan dengan penelitian yang menggunakan aliran nitrogen pada larutan pra-polimer, kemudian diletakkan di dalam water bath atau oil bath [8,17]. ...
Molecularly Imprinted Polymer (MIP) of melamine has been made using cooling-heating method. Melamine as the template is inserted into the solvent (ethanol + aquabidest), then added functional monomer (methacrylic acid), a cross-linker (ethylene glycol dimethacrylate), and an initiator (benzoyl peroxide). The pre-polymer solution was cooled in a refrigerator at -5ºC for an hour, and was heated in an oven at 75°C for 7 hours. The time is required to create a solid polymer MIP melamine with cooling-heating method is more efficient than the method use nitrogen flowing in the pre-polymer solution and then is put in a water bath and exposed to UV. Template in the polymer particles is removed by washing the polymer particles repeatedly to increase the effectiveness of cavities formation. Furthermore, MIP characterized use FTIR. The FTIR results show that the absorbance at 1000-1360 cm-1 wave number which is characteristic of the amine group wave number, for the unwashed polymer has a higher peak of 0,25 is compared with melamine MIP of 0,14. Keywords: MIP, melamine, cooling-heating, FTIR
Diazepam is a benzodiazepine class usage is regulated nationally or globally. These drugs can be used to regulate sleep patterns or sedative-hypnotic drugs because it has a calming effect. Monitoring the abuse of diazepam requires a sensitive analysis methods that required the preparation of selective methods. One of the methods that are currently developing is Moleculary Imprinted Polymer-Solid Phase Extraction (MI-SPE). In this research, step being performed include determination of the association constant, synthesis sorbent of Imprinted Polymer (IP) diazepam by bulkpolymerization method with diazepam as a template, chloroform as porogen, two kind of monomer methacrylic acid (MAA) and hydroxyethyl methacrylate (HEMA) as functional monomer. Templates extracted from polymer followed by evaluation of adsorption ability test, a test of capacity and selectivity of the polymer, and also the characterization of the IP using Fourier Transform Infra-Red (FTIR),and Scanning Electron Microscope (SEM). The results showed that IP diazepam with MAA monomer has 7.95 x 10-5 mg/g of capacity, it is better than capacity of IP diazepam monomer HEMA with 7.47x 10-6 mg/g. Selectivity of IP diazepam MAA monomer has an IF value which is 2.13, which is better than IP HEMA with 1.21. In addition, IP diazepam MAA monomer more heterogenous than its Non Imprinted Polymer (NIP).Keywords: Chloroform, Diazepam, HEMA, Methacrylic acid, MI-SPE.
Molecularly Imprinted Polymer (MIP) has been synthesized with carbaryl used as a template and forms complex bonds with Methacrylic Acid (MAA)through hydrogen bonds, followed by a cross-linking process using Ethylene Glycol Dimethacrylate (EGDMA) cross-linkers. The polymerization process begins with the thermal decomposition of Benzoyl Peroxide (BPO) as an initiator. Non-Imprinted Polymer (NIP) as a control polymer has also been synthesized using a similar procedure without using carbaryl templates. In this study, two variations of carbaryl are used, which are not milled carbamates, and carbaryl has been milled using High Energy Milling (HEM). The FTIR study was carried out to investigate the presence of carbaryl in polymers, MIP, and NIP. The spectrum shows that the concentration of carbaryl compound decreases after the extraction process. This result was also confirmed by the increase in the value of the percentage of transmittance in the MIP, especially the nano carbaryl MIP. This result is supported by the X-RD results, which showed a decrease in the size of the crystals in the carbaryl MIP from 10.07 Å while the nano carbaryl MIP was 9.16 Å.
