scholarly journals Interações químicas entre monômero e molécula molde em polímeros com impressão molecular, o EGDMA: 2-VP (4: 1) - estudo de caso MIP lumefantrina

2021 ◽  
Vol 4 (04) ◽  
pp. 56-76
Author(s):  
Maria Betânia de Freitas-Marques ◽  
Wagner da Nova Mussel1 ◽  
Maria Irene Yoshida ◽  
Christian Fernandes ◽  
Tércio Assunção Pedros ◽  
...  

Molecularly Imprinted Polymers (MIP) are synthetic materials used as a tool to enhance the selectivity in different analytical approaches, such as solid-phase extraction, chromatography, and sensing devices. Knowing the mechanism involved in the interaction between the template and monomer is essential for a further successful application. However, studies on this topic are scarce. This work evaluates the involved mechanisms in the template-monomer interaction for a lumefantrine MIP system, an antimalarial drug. Field-emission gun scanning electron microscopy, thermal analysis, X-ray diffraction, and density functional theory were applied to determine the mechanism involved in two MIPs obtained in different conditions. A new parameter, named Molecularly Imprinting Factor (MIF), was proposed to evaluate the contribution of specific interactions in the sorption of the analyte by the MIP structure. MIF allows direct insights into specific binding, non-specific contributions, interaction nature, behavior predictability, system acid-base behavior, pre-screening pairs capability, and binding site affinities evaluation. Two interaction types were observed, covalent and non-covalent, when methacrylic acid and 2-vinyl pyridine were used as monomers, respectively. Therefore, the use of methacrylic acid formed a sorbent inappropriate for solid-phase extraction since the binding is not reversible. On the other hand, 2-vinyl pyridine-lumefantrine binding was reversible, and MIF = 0.59 (59.02% of specific site sorption) indicates that the predominant mechanism in the sorption is specific.

Author(s):  
Sophi Damayanti ◽  
Untung Gunawan ◽  
Slamet Ibrahim

Background: The use of nitrofurantoin and other nitrofuran antibiotics in food which produced from animals is prohibited by European Union because of potentially carcinogenic and mutagenic. Various methods for analysis of residues of nitrofurantoin has been developed, but because of the interference of the matrix, it is necessary to separate the matrix therefore, the matrix effect will not interfere the analysis. Nowadays, molecular imprinted polymer (MIP) is a well-developed tool in the analytical field, mainly for separating substances in relatively complex matrices.Objective: The purpose of this study is to obtain MISPE that is selective for the separation of nitrofurantoin residues in chicken eggs.Methods: Analytical methods development of nitrofurantoin were optimization of HPLC system and validation of analytical methods performed to obtain the suitable system for nitrofurantoin detection. In silico study used for MIP design by observing the difference Gibbs free energy using Gaussview 5.08 software with Density Functional Theory (DFT) methods using 6-311G as basis set. MIP synthesis was done using bulk method use nitrofurantoin as template, acrylamide as functional monomer, ethyleneglycoldimethacrylate (EGDMA) as crosslinker, and azobisisobutyronitrile (AIBN) as an initiator reaction inside dimethylformamide (DMF) as solvent. Non imprinted polymer (NIP) was synthesized as comparison. MIP and NIP which has been synthesized was inserted into SPE cartridge and characterized using Infrared spectroscopy and HPLC.Result: MISPE that has been synthesized was characterized and compared to non-imprinted polymer solid phase extraction (NISPE) and marketed Solid Phase Extraction (SPE) C18. Sensitivity of MIP, NIP, and SPE C-18 to nitrofurantoin was 84.54 %, 37.73 %, and 33.95 % respectively, based on recovery of nitrofurantoin.Conclusion: Based on the result it was obtained MISPE has high selectivity toward nitrofurantoin compared to NISPE and either marketed SPE.  


2013 ◽  
Vol 781-784 ◽  
pp. 1359-1365 ◽  
Author(s):  
Yin Zhe Jin ◽  
Yun Zhe Jin ◽  
Ji Yu Piao ◽  
Ying Shan Jin ◽  
Yong Hao Xuan

Recently, molecularly imprinted solid phase extraction (MISPE) has been used more frequently separate drugs and natural substances. This modern separation methodologies require reliable tools that perform on a high level in terms of efficiency and reproducibility. The molecular imprinting technique is a reliable technique for the preparation of materials of predetermined selectivity. It is highly significant in research of the structure of enzyme, mechanism of receptor-antibody and analytical chemistry. Solid phase extraction can be used to isolate and pre-concentrate the analytes in complex samples. This technique is more rapid, simple, economical and environment-friendly than the traditional liquid-liquid extraction. The materials used in SPE are usually based on the non-specific binding of the targets, which often suffers some shortcomings, such as low specificity and selectivity. In recent years, solid phase extraction involving molecular imprinted polymer have been proved to be successful applications for its features of high selectivity, ease of synthesis, low cost for preparation and workability under different conditions especially that of harsh pH and organic solvents. In this work, the principles, application and development tends of MISPE will be reviewed and the disadvantages and limitation of the MISPE and future development direction are also briefly discussed.


2014 ◽  
Vol 665 ◽  
pp. 311-314
Author(s):  
Qing Shan Liu ◽  
Xu Li ◽  
Shu Juan Zhuang ◽  
Wei Wei Zhang ◽  
Xiao Ying Yin ◽  
...  

Molecular imprinting technology (MIT) is a developing technique with high recognition which is just like the recognition between enzymes and antibodies in the organism. Molecularly imprinted polymers (MIPs), synthetic materials obtained using the imprinting technology, have played a huge advantage and been used in many fields. Especially, MIPs have been applied to the extraction and separation of analytes as the selective adsorbent of solid-phase extraction (SPE), which is known as molecularly imprinted polymer solid-phase extraction (MISPE) in recent years. In the present review, the methodology of MIPs preparation and evaluation are explained. Moreover, recent great developments of SPE and MISPE are discussed, and the potential application of MISPE in extraction of traditional Chinese medicine (TCM) active ingredients are also presented briefly.


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.


Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2924
Author(s):  
Karen A. Escamilla-Lara ◽  
Ana C. Heredia ◽  
Araceli Peña-Alvarez ◽  
Israel S. Ibarra ◽  
Enrique Barrado ◽  
...  

A magnetic solid phase extraction technique followed by liquid chromatography with a fluorescence detector for naproxen analysis in human urine samples was developed. The method includes the extraction of naproxen with a magnetic solid synthetized with magnetite and poly 4-vinylpriridine, followed by the magnetic separation of the solid phase and desorption of the analyte with methanol. Under optimal conditions, the linear range of the calibration curve was 0.05–0.60 μg L−1, with a limit of detection of 0.02 μg L−1. In all cases values of repeatability were lower than 5.0% with recoveries of 99.4 ± 1.3%. Precision and accuracy values are adequate for naproxen (Npx) analysis in urine samples.


2019 ◽  
Vol 46 (3) ◽  
pp. 3063-3072
Author(s):  
Petr Šálek ◽  
Marcela Filipová ◽  
Daniel Horák ◽  
Vladimír Proks ◽  
Olga Janoušková

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