Synthesis and characterization of poly(styrene-co-divinylbenzene) and nanomagnetite structures.

The use of iron oxide nanoparticles for the synthesis of adsorbents materials with application in contaminated water remediation is based on both their magnetic and adsorption properties. Poly(styrene-co-divinylbenzene) - Poly(Sty-co-DVB)microparticles are widely known for this use and the addition of magnetite comes to add magnetic properties, however it should not limit the functionalization processes for formation of cationic and/or anionic resins. Thus, there is a concern about the stability of magnetite in acidic environments, as required by the sulfonation process, for example. Furthermore, the synthesis of composites with magnetic nanoparticles is a challenge due to the strong magnetic dipole interactions between particles resulting from the high specific surface area, making them susceptible to aggregation. As well as oxidation during the synthesis process can compromise the structure of the initial magnetic material. In this sense, the present work validated processes for the synthesis of Poly(Sty-co-DVB)/magnetite microparticles that sought, as a final result, the incorporation of magnetite aiming to preserve its initial structural conformation. Thus, started from original synthesis method aimed at the production of Poly(Sty-co-DVB) microparticles without magnetite, to methods in which magnetite nanoparticles is added through two distinct processes, different regarding the use or not of oleic acid in its preparation. In this method article we show:•Combination of methods to preserve the structure of magnetite in the Poly(Sty-co-DVB)/magnetite composite.•Simple method of adding magnetite to the Poly(Sty-co-DVB)/magnetite composite synthesis process.•Magnetite treatment method with oleic acid in Poly(Sty-co-DVB)/magnetite composite synthesis. The samples were characterized using Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and Mössbauer spectroscopy to evaluate the chemical modifications that were introduced in the original synthesis method.

Synthesis and characterization of a molecularly imprinted polymer (MIP) for solid-phase extraction of the antidiabetic gliclazide from human plasma.

Gliclazide is a sulfonylurea frequently prescribed for the management of type 2 diabetes mellitus in elderly patients and for patients with chronic renal or hepatic diseases. Even though it is considered a safer alternative, the drug can provoke side effects in some patients, especially hypoglycemia, due to the high interindividual variability. Therefore, the quantification of gliclazide in biological samples is usually recommended in order to assure efficacy and safety of the pharmacotherapy. However, due to the complexity of biological matrices, therapeutic monitoring can be very challenging, especially in the sample preparation step. For that reason, the synthesis and characterization of a novel and selective molecularly imprinted polymer (MIP) was proposed to be employed as sorbent for the extraction of gliclazide from human plasma samples by a molecularly imprinted solid-phase extraction (MISPE) procedure. Synthesis conditions were optimized (monomer, crosslinker and porogen) and the polymer was characterized for its morphological, physicochemical and stability properties. The influence of drug concentration, solvent composition and pH on the coefficient of distribution (Kd) and imprinting factor (IF) were studied, as well as repeatability between batches and selectivity. A bioanalytical method was developed applying the developed MIP as sorbent in solid phase extraction and liquid chromatography using a Poroshell 120 C18 (100 × 4.6 mm, 4 µm) column, acetonitrile and 10 mM potassium phosphate buffer pH 3.0 (50:50) at a flow-rate of 1.2 mL/min as mobile phase, temperature of 30 °C, injection volume of 40 µL and detection at 230 nm. The best reaction yield, extraction capacity, and selectivity was obtained using 2-hydroxyethyl methacrylate (2-HEMA), ethyleneglycol dimethacrylate (EGDMA) and acetonitrile. The optimized MIP showed coefficient of distribution (Kd) of 59.85 µg/g, imprinting factor (IF) of 1.60, and selectivity for gliclazide and other sulfonylureas compared to possible concurrent drugs. The developed method by MISPE-HPLC-UV showed to be appropriate to determine gliclazide in human plasma samples.

Molecularly imprinted polymer for determination of lumefantrine in human plasma through chemometric-assisted solid-phase extraction and liquid chromatography.

Lumefantrine is the first-choice treatment of Falciparum uncomplicated malaria. Recent findings of resistance to lumefantrine has brought attention for the importance of therapeutic monitoring, since exposure to subtherapeutic doses of antimalarials after administration is a major cause of selection of resistant parasites. Therefore, this study focused on the development of innovative, selective, less expensive and stable molecularly imprinted polymers (MIPs) for solid-phase extraction (SPE) of lumefantrine from human plasma to be used in drug monitoring. Polymers were synthesized by precipitation polymerization and chemometric tools (Box-Behnken design and surface response methodology) were employed for rational optimization of synthetic parameters. Optimum conditions were achieved with 2-vinylpyridine as monomer, ethylene glycol dimethacrylate as crosslinker and toluene as porogen, at molar ratio of 1:6:30 of template/monomer/crosslinker and azo-bisisobutyronitrile as initiator at 65 °C. The MIP obtained was characterized and exhibited high thermal stability, adequate surface morphology and porosity characteristics and high binding properties, with high affinity (adsorption capacity of 977.83 µg g-1) and selectivity (imprinting factor of 2.44; and selectivity factor of 1.48 and selectivity constant of 1.44 compared with halofantrine). Doehlert matrix and fractional designs were satisfactorily used for development and optimization of a MISPE-HPLC-UV method for determination of lumefantrine. The method fulfilled all validation parameters, with recoveries ranging from 83.68% to 85.42%, and was applied for quantitation of the drug in plasma from two healthy volunteers, with results of 1407.89 and 1271.35 ng mL-1, respectively. Therefore, the MISPE-HPLC-UV method optimized through chemometrics provided a rapid, highly selective, less expensive and reproducible approach for lumefantrine drug monitoring.

Synthesis and Characterization of Poly(N-isopropylacrylamide)/SBA-15 Silica Nanocomposites.

The combination of the mesoporous silica material SBA-1 5 with the temperature-responsive hydrogels, such as poly(N-isopropylacrylamide) P(N-iPAAm) can lead to the formation of a material with the potential for application as a new drug delivery system, given that self-regulated delivery allows for drug release when needed. The present work studies the synthesis and characterization of hybrid systems consisting of the poly(N-isopropylacrylamide) hydrogel and SBA-15 by varying the amount of hydrogel within the silica network. A systematic study on the structural properties of hybrid samples, their thermal stability and the degradation of the polymer chains in silica was carried out through characterization techniques, including SAXS, thermogravimetry and physical adsorption of N2. The results were critically examined and compared with pure SBA-15. The present study's results demonstrated that the thermosensibility of P(N-iPAAm) was retained in the hybrid system, which presented a low critical solution temperature, similar to that of pure P(N-iPAAm). Moreover, the hydrogel did not fully occupy the available intrachannel space, making the [SBA-15/P(N-iPAAm)] hybrids a very promising candidate for hosting and further delivery, under appropriate conditions, of a variety of molecules of pharmaceutical interest.