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1.
Electrophoresis ; 2024 Aug 09.
Artigo em Inglês | MEDLINE | ID: mdl-39126162

RESUMO

Dielectrophoresis (DEP) is an electrokinetic effect first studied in the early 20th century. Since then, DEP has gained significant interest in research, owing to its ability to solve particle separation problems in various industries. Dielectrophoretic filtration (DEP filtration) is a separation method using DEP to filter a wide range of microparticles, from bacterial cells to catalytic particles. DEP filtration can selectively separate particles based on size or dielectric properties, recover trapped particles and avoid common problems associated with mechanical filtration based on pore size (e.g. pressure drops and regular filter replacements). This review describes the simple beginnings of DEP filtration and how our understanding and applications for DEP filtration have progressed over time. A brief section of DEP theory as well as a note on the general outlook for DEP filtration in the future is presented. DEP filtration offers an exciting opportunity to selectively separate diverse particle mixtures. To achieve such a feat, technical challenges such as Joule Heating and low throughputs must be addressed.

2.
Chirality ; 36(2): e23632, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-37994273

RESUMO

The R,S-enantiomer impurity and diastereomer impurities (S,S-isomer and R,R-isomer) of the solifenacin (S,R-enantiomer) were effectively separated and quantified simultaneously utilizing normal-phase high-performance liquid chromatography with a chiral stationary phase consisting of amylose tris (3,5-dimethylphenylcarbamate) coated on silica-gel (Chiralpak, AD-H). The enantiomeric and stereo-selective separation was achieved within a run time of 35 minutes using a mobile phase of 'n-hexane, ethanol, and diethylamine' in an isocratic elution mode with a detection wavelength of 220 nm. The validation attributes assessed were accuracy (which showed excellent recoveries between 97.5% and 100.4%) and linearity (which was proven in the range of 0.081-1.275 µg.mL-1 , with a linear regression of 0.999). The stress testing experiments proved that the developed methodology by the HPLC technique has stability-indicating characteristics, as all closely eluting peak pairs were separated well with a resolution of 2.3 and without any interference. The proposed methodology was highly efficient in separating and simultaneously determining the chiral impurities (enantiomers and diastereomers) of the solifenacin in the release and stability sample analyses of drug substances and tablets in pharmaceutical formulations.


Assuntos
Amilose , Fenilcarbamatos , Succinato de Solifenacina , Cromatografia Líquida de Alta Pressão/métodos , Amilose/química , Estereoisomerismo , Receptores Muscarínicos
3.
Molecules ; 29(16)2024 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-39202947

RESUMO

A traditional phase transformation method is commonly used to prepare molecular imprinting membranes for selective separation. However, traditional molecularly imprinted polymers are mostly micron-sized particles, and the imprinting sites in their membrane are easily embedded, leading to a reduced adsorption capacity and decreased selectivity. In this study, an ultra-long nanowire with a diameter of about 15 nm was synthesized for the separation of artemisinin (ART), and its adsorption capacity was as high as 198.29 mg g-1 after imprinting polymerization. Molecular imprinting membranes were prepared, using polyvinylidene fluoride (PVDF), polyethersulfone (PES), and polysulfone (PSF) as the membrane matrix, for comparison. The average membrane pore size of PVDF-MIM was about 480 nm, and PVDF-MIM had the highest adsorption capacity (69 mg g-1) for ART. The optimal flow rate for PVDF-MIM's dynamic adsorption of ART was 7 mL min-1. Under this optimal flow rate, selectivity experiments were carried out to obtain the separation factor of PVDF-MIM (α = 8.37), which was much higher than the corresponding values of PES-MIM and PSF-MIM. In addition, the hydrophobicity and low flux of PES-MIM and PSF-MIM lead to higher non-specific adsorption. The hydrophobicity of PVDF-MIM is lower than that of PES-MIM and PSF-MIM, which greatly reduces the non-specific adsorption of the membrane, thus increasing the selectivity of the membranes. Therefore, the effective density of the imprinting sites in the pores and the membrane structure are the main factors determining the efficient separation of molecularly imprinted membranes.

4.
Angew Chem Int Ed Engl ; 63(39): e202407278, 2024 Sep 23.
Artigo em Inglês | MEDLINE | ID: mdl-38924343

RESUMO

The concept of pore space partition has emerged as an effective strategy for developing improved coordination-based supramolecular porous materials with exceptional performance. Herein, we report that a water-soluble self-assembled tetrahedral cage 1 with a partitioned cavity shown excellent performance as a multifunctional extractant. The results show that this unique partitioned cavity can efficiently separate halogenated adamantanes, adamantane isomers, and polycyclic aromatic hydrocarbons. Furthermore, the influence of cavity-partitioned cage 1 on the electrochemical properties of redox-active molecules and electrochemically driven reversible host-guest process has also been demonstrated. The findings offer valuable insights into the design and development of new type of materials with controlled phase separation and tailored electrochemical properties.

5.
Small ; 19(24): e2208212, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-36916691

RESUMO

137 Cs and 90 Sr are hazardous to ecological environment and human health due to their strong radioactivity, long half-life, and high mobility. However, effective adsorption and separation of Cs+ and Sr2+ from acidic radioactive wastewater is challenging due to stability issues of material and the strong competition of protons. Herein, a K+ -activated niobium germanate (K-NGH-1) presents efficient Cs+ /Sr2+ coadsorption and highly selective Cs+ /Sr2+ separation, respectively, under different acidity conditions. In neutral solution, K-NGH-1 exhibits ultrafast adsorption kinetics and high adsorption capacity for both Cs+ and Sr2+ (qm Cs  = 182.91 mg g-1 ; qm Sr  = 41.62 mg g-1 ). In 1 M HNO3 solution, K-NGH-1 still possesses qm Cs of 91.40 mg g-1 for Cs+ but almost no adsorption for Sr2+ . Moreover, K-NGH-1 can effectively separate Cs+ from 1 M HNO3 solutions with excess competing Sr2+ and Mn + (Mn +  = Na+ , Ca2+ , Mg2+ ) ions. Thus, efficient separation of Cs+ and Sr2+ is realized under acidic conditions. Besides, K-NGH-1 shows excellent acid and radiation resistance and recyclability. All the merits above endow K-NGH-1 with the first example of niobium germanates for radionuclides remediation. This work highlights the facile pH control approach towards bifunctional ion exchangers for efficient Cs+ /Sr2+ coadsorption and selective separation.

6.
Environ Sci Technol ; 57(38): 14464-14471, 2023 09 26.
Artigo em Inglês | MEDLINE | ID: mdl-37706485

RESUMO

Nanofiltration (NF) is a promising and sustainable process to extract Li+ from brine lakes with high Mg2+/Li+ mass ratios. However, a trade-off between Li/Mg selectivity and Li recovery exists at the process scale, and the Li/Mg selectivity of commercially and lab-made NF membranes in a single-pass NF process is insufficient to achieve the industrially required Li purity. To overcome this challenge, we propose a multipass NF process with brine recirculation to achieve high selectivity without sacrificing Li recovery. We experimentally demonstrate that Li/Mg selectivity of a three-pass NF process with a commercial NF membrane can exceed 1000, despite the compromised Li recovery as a result of co-existing cations. Our theoretical analysis further predicts that a four-pass NF process with brine recirculation can simultaneously achieve an ultrahigh Li/Mg selectivity of over 4500 and a Li recovery of over 95%. This proposed process could potentially facilitate efficient NF-based solute-solute separations of all kinds and contribute to the development of novel membrane-based separation technologies.


Assuntos
Lítio , Sais , Íons , Tecnologia
7.
Macromol Rapid Commun ; 44(11): e2200718, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-36271740

RESUMO

High-performance membranes are critical to membrane separation technology. In recent years, 2D covalent organic frameworks (2D COFs) have attracted extensive attention in the field of membrane separation due to their high porosity, ordered channels, and fine-tuned pore sizes, which are considered as excellent candidate to solve the trade-off between membrane selectivity and permeability. Herein, two kinds of ionic 2D COFs with different charge properties (termed as iCOFs) are integrated into polyacrylonitrile (PAN) substrates to form two composite membranes (PAN@iCOFs) with excellent selective perfluoroalkyl substances (PFASs) separation performance with high solvent permeability and good mechanical properties. The as-prepared PAN@iCOFs composite membranes can selectively reject more than 99.0% of positively and negatively charged PFASs in wastewater while maintaining good stability and recyclability.


Assuntos
Fluorocarbonos , Estruturas Metalorgânicas , Íons , Membranas , Permeabilidade
8.
Environ Res ; 218: 114987, 2023 02 01.
Artigo em Inglês | MEDLINE | ID: mdl-36462694

RESUMO

Selective separation of nitrate over chloride is crucial for eutrophication mitigation and nitrogen resource recovery but remains a challenge due to their similar ionic radius and the same valence. Herein, a polypyrrole membrane electrode (PME) was fabricated by polymerization of pyrrole (Py) and p-toluenesulfonate (pTS), which was used as a working electrode in redox transistor electrodialysis. The anions in the source solution were first incorporated into the PME at reduction potentials and then released to receiving solution at oxidation potentials. Pulse widths and potentials were optimized to maximize the ion separation performance of PME, resulting in the improvement of NO3-/Cl- separation factor up to 6.93. The ion distributions in various depths of PME indicated that both NO3- and Cl- were incorporated into PME at negative potentials. Then, NO3- was preferentially released from PME at positive potentials, but most Cl- was retained. This was ascribed to the high binding energy between Cl- and PPy/pTS structure, which was 51.4% higher than that between NO3- and PPy/pTS structure. Therefore, the higher transport rate of NO3- in comparison with Cl- was achieved, leading to a high NO3- selectivity over Cl-. This work provides a promising avenue for the selective separation of nitrate over chloride, which may contribute to nitrogen resource recycling and reuse.


Assuntos
Cloretos , Nitratos , Polímeros/química , Pirróis/química , Ânions , Eletrodos , Oxirredução
9.
Molecules ; 28(21)2023 Nov 06.
Artigo em Inglês | MEDLINE | ID: mdl-37959871

RESUMO

In this study, a new 3D porous PVDF-foam-imprinted membrane (PPIM) for the selective separation of artemisinin (ART) was first prepared via the dopamine adhesion of pre-synthesized MIPs into the interior of the PPIM. In the PPIM, the pre-synthesized molecularly imprinted polymers (MIPs) with artesunate (ARU) as a dummy template were uniformly loaded on the interior of the membrane, avoiding the defects of recognition site encapsulation found in the conventional membrane. This membrane also exhibited excellent flux, which is beneficial in practical separation applications. The PPIM was systematically characterized via FT-IR, SEM, pore-size distribution analysis, water contact angle test, membrane flux, and mechanical performance analysis, respectively. In the static adsorption experiment, the pseudo-second-order kinetic model better fitted the rebinding data of ART. Under dynamic conditions, the ART adsorption capacity of the PPIM could be further remarkably improved by tailoring the flow rate to 3 mL min-1. In the selective separation experiment, with artemether (ARE) as the competition substrate, the selective separation ability (α) of the PPIM towards ART/artemether (ARE) reached its peak value (3.16) within only 10 min at this flow rate, which is higher than that of porous PVDF foam non-imprinted membranes (PPNM) (ca. 1.5), showing great separation efficiency in a short time. Moreover, the PPIM can be reused five times without a significant decrease in its adsorption capacities, showing good regeneration performance. This work highlights a simple strategy for constructing new MIMs with high flux and great mechanical strength to achieve the efficient selective separation of ART and ARE in practical applications.

10.
Molecules ; 28(15)2023 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-37570733

RESUMO

Molecularly imprinted membranes (MIMs), the incorporation of a given target molecule into a membrane, are generally used for separating and purifying the effective constituents of various natural products. They have been in use since 1990. The application of MIMs has been studied in many fields, including separation, medicine analysis, solid-phase extraction, and so on, and selective separation is still an active area of research. In MIM separation, two important membrane performances, flux and permselectivities, show a trade-off relationship. The enhancement not only of permselectivity, but also of flux poses a challenging task for membranologists. The present review first describes the recent development of MIMs, as well as various preparation methods, showing the features and applications of MIMs prepared with these different methods. Next, the review focuses on the relationship between flux and permselectivities, providing a detailed analysis of the selective transport mechanisms. According to the majority of the studies in the field, the paramount factors for resolving the trade-off relationship between the permselectivity and the flux in MIMs are the presence of effective high-density recognition sites and a high degree of matching between these sites and the imprinted cavity. Beyond the recognition sites, the membrane structure and pore-size distribution in the final imprinted membrane collectively determine the selective transport mechanism of MIM. Furthermore, it also pointed out that the important parameters of regeneration and antifouling performance have an essential role in MIMs for practical applications. This review subsequently highlights the emerging forms of MIM, including molecularly imprinted nanofiber membranes, new phase-inversion MIMs, and metal-organic-framework-material-based MIMs, as well as the construction of high-density recognition sites for further enhancing the permselectivity/flux. Finally, a discussion of the future of MIMs regarding breakthroughs in solving the flux-permselectivity trade-off is offered. It is believed that there will be greater advancements regarding selective separation using MIMs in the future.

11.
Molecules ; 28(20)2023 Oct 12.
Artigo em Inglês | MEDLINE | ID: mdl-37894522

RESUMO

Nucleoside analogs play a crucial role in the production of high-value antitumor and antimicrobial drugs. Currently, nucleoside analogs are mainly obtained through nucleic acid degradation, chemical synthesis, and biotransformation. However, these methods face several challenges, such as low concentration of the main product, the presence of complex matrices, and the generation of numerous by-products that significantly limit the development of new drugs and their pharmacological studies. Therefore, this work aims to summarize the universal separation methods of nucleoside analogs, including crystallization, high-performance liquid chromatography (HPLC), column chromatography, solvent extraction, and adsorption. The review also explores the application of molecular imprinting techniques (MITs) in enhancing the identification of the separation process. It compares existing studies reported on adsorbents of molecularly imprinted polymers (MIPs) for the separation of nucleoside analogs. The development of new methods for selective separation and purification of nucleosides is vital to improving the efficiency and quality of nucleoside production. It enables us to obtain nucleoside products that are essential for the development of antitumor and antiviral drugs. Additionally, these methods possess immense potential in the prevention and control of serious diseases, offering significant economic, social, and scientific benefits to the fields of environment, biomedical research, and clinical therapeutics.


Assuntos
Impressão Molecular , Nucleosídeos , Polímeros/química , Impressão Molecular/métodos , Polímeros Molecularmente Impressos , Cromatografia Líquida de Alta Pressão/métodos , Adsorção , Extração em Fase Sólida/métodos
12.
Molecules ; 26(16)2021 Aug 19.
Artigo em Inglês | MEDLINE | ID: mdl-34443623

RESUMO

Phenolic compounds have long been of great importance in the pharmaceutical, food, and cosmetic industries. Unfortunately, conventional extraction procedures have a high cost and are time consuming, and the solvents used can represent a safety risk for operators, consumers, and the environment. Deep eutectic solvents (DESs) are green alternatives for extraction processes, given their low or non-toxicity, biodegradability, and reusability. This review discusses the latest research (in the last two years) employing DESs for phenolic extraction, solvent components, extraction yields, extraction method characteristics, and reviewing the phenolic sources (natural products, by-products, wastes, etc.). This work also analyzes and discusses the most relevant DES-based studies for phenolic extraction from natural sources, their extraction strategies using DESs, their molecular mechanisms, and potential applications.


Assuntos
Produtos Biológicos/química , Fracionamento Químico/métodos , Fenóis/isolamento & purificação , Solventes/química
13.
Angew Chem Int Ed Engl ; 60(35): 19047-19052, 2021 Aug 23.
Artigo em Inglês | MEDLINE | ID: mdl-34288296

RESUMO

Two-dimensional covalent organic frameworks (2D COFs) are considered as potential candidates for gas separation membranes, benefiting from permanent porosity, light-weight skeletons, excellent stability and facilely-tailored functionalities. However, their pore sizes are generally larger than the kinetic diameters of common gas molecules. One great challenge is the fabrication of single-phase COF membranes to realize precise gas separations. Herein, three kinds of high-quality ß-ketoenamine-type COF nanosheets with different pore sizes were developed and aggregated to ultrathin nanosheet membranes with distinctive staggered stacking patterns. The narrowed pore sizes derived from the micro-structures and selective adsorption capacities synergistically endowed the COF membranes with intriguing CO2 -philic separation performances, among which TpPa-2 with medium pore size exhibited an optimal CO2 /H2 separation factor of 22 and a CO2 permeance of 328 gas permeation units at 298 K. This membrane performance reached the target with commercial feasibility for syngas separations.

14.
Angew Chem Int Ed Engl ; 59(3): 1161-1165, 2020 Jan 13.
Artigo em Inglês | MEDLINE | ID: mdl-31724807

RESUMO

Covalent organic frameworks (COFs) have attracted attention due to their ordered pores leading to important industrial applications like storage and separation. Combined with their modular synthesis and pore engineering, COFs could become ideal candidates for nanoseparations. However, the fabrication of these microcrystalline powders as continuous, crack-free, robust films remains a challenge. Herein, we report a simple, slow annealing strategy to construct centimeter-scale COF films (Tp-Azo and Tp-TTA) with micrometer thickness. The as-synthesized films are porous (SABET =2033 m2 g-1 for Tp-Azo) and chemically stable. These COFs have distinct size cut-offs (ca. 2.7 and ca. 1.6 nm for Tp-Azo and Tp-TTA, respectively), which allow the size-selective separation of gold nanoparticles. Unlike, other conventional membranes, the durable structure of the COF films allow for excellent recyclability (up to 4 consecutive cycles) and easy recovery of the gold nanoparticles from the solution.

15.
J Sep Sci ; 42(6): 1265-1272, 2019 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-30653834

RESUMO

Cyclitols and sugars were obtained as a mixture from Medicago sativa L., in a comparative study by using maceration, and pressurized liquid extraction, as a modern and green extraction techniques. The influence of extraction parameters including: extraction temperature, time and number of cycles on the content of sugars and cyclitols was investigated based on response surface methodology. The highest total amount of sugars and cyclitols (62.27 ± 2.30 and 50.35 ± 0.77 mg/g of dry material, respectively) was obtained when extraction was performed at 88°C, for 22 min, in two cycles. The methodology used involved extraction, purification, selective separation (using yeast and anion exchange resin) and derivatization, followed by gas chromatography -mass spectrometry analysis. The use of yeast treatment realized an effective fractionation of cyclitols and sugars, which allowed the removal of most sugars. The involvement of anion exchange resin after yeast allowed the removal of sugar alcohols and lactose, together with other sugar traces remained and to obtain a solution containing six cyclitols. The recrystallization of dry residue after solvent evaporation, from ethanol, allowed us to obtain 14.65 mg of white pure crystals identified with NMR spectroscopy, liquid chromatography with mass spectrometry, gas chromatography with mass spectrometry, optical rotation and melting point as analysis D-pinitol.


Assuntos
Ciclitóis/isolamento & purificação , Extração Líquido-Líquido , Medicago sativa/química , Açúcares/isolamento & purificação , Temperatura , Configuração de Carboidratos , Ciclitóis/química , Pressão , Açúcares/química , Propriedades de Superfície , Fatores de Tempo
16.
Int J Mol Sci ; 20(8)2019 Apr 20.
Artigo em Inglês | MEDLINE | ID: mdl-31009989

RESUMO

The valorization of by-products from natural organic sources is an international priority to respond to environmental and economic challenges. In this context, electrodialysis with filtration membrane (EDFM), a green and ultra-selective process, was used to separate peptides from salmon frame protein hydrolysate. For the first time, the simultaneous separation of peptides by three ultrafiltration membranes of different molecular-weight exclusion limits (50, 20, and 5 kDa) stacked in an electrodialysis system, allowed for the generation of specific cationic and anionic fractions with different molecular weight profiles and bioactivity responses. Significant decreases in peptide recovery, yield, and molecular weight (MW) range were observed in the recovery compartments depending on whether peptides had to cross one, two, or three ultrafiltration membranes. Moreover, the Cationic Recovery Compartment 1 fraction demonstrated the highest increase (42%) in glucose uptake on L6 muscle cells. While, in the anionic configuration, both Anionic Recovery Compartment 2 and Anionic Recovery Compartment 3 fractions presented a glucose uptake response in basal condition similar to the insulin control. Furthermore, Cationic Recovery Compartment 3 was found to contain inhibitory peptides. Finally, LC-MS analyses of the bioassay-guided bioactive fractions allowed us to identify 11 peptides from salmon by-products that are potentially responsible for the glucose uptake improvement.


Assuntos
Glucose/metabolismo , Peptídeos/isolamento & purificação , Hidrolisados de Proteína/isolamento & purificação , Salmão/metabolismo , Animais , Ânions , Cátions , Linhagem Celular , Diálise , Camundongos , Peso Molecular , Termodinâmica , Ultrafiltração
17.
Molecules ; 24(3)2019 Feb 04.
Artigo em Inglês | MEDLINE | ID: mdl-30720731

RESUMO

Stainless steel wire mesh supported molecularly imprinted composite membranes for selective separation of Ebracteolata Compound B (ECB) were prepared based on surface polymerization using ECB separated from Euphorbia fischeriana as a template, acrylamide as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, azodiisobutyronitrile as an initiator, and stainless steel wire mesh as support. Structure and purity of ECB were characterized by nuclear magenetic resonance (¹H-NMR, 13C-NMR) and ultra high performance liquid chromatography (UHPLC). The molecularly imprinted composite membranes were characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope (SEM). The membrane adsorbed on the ECB reached equilibrium about 30 min later, with a maximum adsorption amount of 3.39 µmol/cm². Adsorption behavior between ECB and the molecularly imprinted composite membranes followed pseudo-second-order kinetics equation and Freundlich isotherm model. The molecularly imprinted composite membranes that could selectively identify and transport ECB in similar structures have a permeation rate of 38.71% to ECB. The ECB content in the permeation solution derived from the extract of Euphorbia fischeriana through the imprinted membrane was 87%. Overall, the obtained results demonstrated that an efficient approach with the molecularly imprinted composite membranes for selective separation of ECB from Euphorbia fischeriana.


Assuntos
Acetofenonas/química , Acetofenonas/isolamento & purificação , Euphorbia/química , Membranas Artificiais , Impressão Molecular/métodos , Aço Inoxidável , Adsorção , Permeabilidade , Polimerização , Polímeros/química , Espectroscopia de Infravermelho com Transformada de Fourier , Aço Inoxidável/química , Temperatura
18.
Electrophoresis ; 2018 Feb 16.
Artigo em Inglês | MEDLINE | ID: mdl-29450897

RESUMO

Two types of molecular-imprinted polymers-based magnetic chitosan with facile deep eutectic solvent-functional monomers (Fe3 O4 -CTS@DES-MIPs) were synthesized and applied as adsorbents in magnetic solid-phase extraction (MSPE) for the selective recognition and separation of (+)-catechin, (-)-epicatechin, and (-)-epigallocatechin gallate in black tea. The obtained Fe3 O4 -CTS@DES-MIPs were characterized by Fourier transform infrared spectroscopy and field emission scanning electron microscopy. The selective recognition ability was examined by adsorption experiments. The actual amounts of (+)-catechin, (-)-epicatechin, and (-)-epigallocatechin gallate extracted from black tea using Fe3 O4 -CTS@DES-MIPs by the MSPE method were 13.10, 6.32, and 8.76 mg/g, respectively. In addition, the magnetic Fe3 O4 -CTS@DES-MIPs showed outstanding recognition and selectivity. Therefore, it can be used to separate bioactive compounds from black tea. The new-type of DES adopted as the functional monomer in this paper provides a new perspective for the recognition and separation of bioactive compounds.

19.
J Sep Sci ; 41(17): 3459-3466, 2018 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-29989660

RESUMO

In this study, a highly sensitive and selective sample pretreatment procedure using molecularly imprinted silica nanoparticles was developed for the extraction and determination of quercetin in red wine samples coupled with high-performance liquid chromatography with ultraviolet detection. The imprinted silica nanoparticles were prepared in the presence of N-acryoyl-l-aspartic acid (functional monomer), quercetin (template), azobisisobutyronitrile (initiator) and methylene bisacrylamide (cross-linker) and methanol/water (porogen) via surface-initiated reversible addition-fragmentation chain transfer polymerization. Surface characterization was performed and several imprinting parameters were investigated, and the results indicated that adsorption of quercetin on the imprinted silica nanoparticles followed a pseudo-first-order adsorption isotherm with a maximum adsorption capacity at 26.4 mg/g within 60 min. The imprinted silica nanoparticles also showed satisfactory selectivity towards quercetin as compared with its structural analogues. Moreover, the imprinted nanoparticles preserved their recognition ability even after five adsorption-desorption cycles. Meanwhile, the nanoparticles were successfully applied to selective extraction of quercetin from red wine with a high recovery (99.7-100.4%). The limit of detection was calculated to be 0.058 µg/mL with a correlation coefficient 0.9996 in the range of 0.2-50 µg/mL. As a result, the developed selective extraction method using molecular imprinting technology simplifies the sample pretreatment procedure before determination of quercetin in real samples.


Assuntos
Impressão Molecular , Nanopartículas/química , Quercetina/análise , Raios Ultravioleta , Vinho/análise , Adsorção , Cromatografia Líquida de Alta Pressão , Estrutura Molecular , Espectrofotometria Ultravioleta
20.
J Sep Sci ; 41(14): 2952-2960, 2018 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-29813175

RESUMO

Magnetic molecularly imprinted nanoparticles were prepared through surface-initiated reversible addition fragmentation chain transfer polymerization by using metronidazole as a template. The molecularly imprinted magnetic nanoparticles were characterized by attenuated total reflection Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, X-ray diffraction, and vibrating sample magnetometry. The adsorption characteristics were also investigated and the kinetics of the adsorption of metronidazole on the imprinted nanoparticles were described by the second-order kinetic model with the short equilibrium adsorption time (30 min). The adsorption isotherm was well matched with the Langmuir isotherm in which the maximum adsorption capacity was calculated to be 40.1 mg/g. Furthermore, the imprinted magnetic nanoparticles showed good selectivity as well as reusability even after six adsorption-desorption cycles. The imprinted magnetic nanoparticles were used as a sorbent for the selective separation of metronidazole from human serum. The recoveries of metronidazole from human serum changed between 97.5 and 99.8% and showed similar sensitivity as an enzyme-linked immunoassay method. Therefore, the molecularly imprinted magnetic nanoparticles might have potential application for the selective and reliable separation of metronidazole from biological fluids in clinical applications.

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