Synthesis and characterization of magnetic molecularly imprinted polymers for the rapid and selective determination of clofazimine in blood plasma samples.

Clofazimine (CLF) is a riminophenazine derivative and a new therapeutic option with high efficacy for patients with rifampicin-resistant tuberculosis (TB). The blood levels of CLF are low and suboptimal, so therapeutic drug monitoring is required. Prior to this study, there were no molecular imprinting-based solid phase extraction (SPE) sorbents that could be used to determine the blood CLF levels. Hence, we prepared a magnetic molecularly imprinted polymer (MMIPs) to capture CLF. We employed computational selection of a functional monomer and crosslinker and confirmed these selections based on the association constant (K a) and a Job plot. We synthesised MMIPs with two surface modifiers and characterized the polymers. Our computational analysis based on the bond energy revealed that methyl methacrylate (MMA) was the most suitable functional monomer at a CLF-to-MMA molar ratio of 1:4. Based on the bond energy, the most suitable crosslinker was trimethylolpropane trimethacrylate (TRIM) at a CLF-to-TRIM molar ratio of 1:1. We determined the K a of MMA and TRIM in different solvents. Isopropanol produced the highest K a. The Job plot showed that a template-to-MMA-to-TRIM molar ratio of 1:4:20 was optimal to synthesize imprinted polymer in isopropanol. We prepared MMIPs using two different modifiers, namely aminopropyltrimethoxysilane (APTES) and oleic acid (OA), using the ratio determined from the Job plot. Physical characteristic tests carried out using FT-IR, SEM-EDS, PSA, BET and VSM, showed that the synthesis was success with a spherical and uniform agglomeration of particles, also a flat surface with many holes with a particle size of MMIP-APTES and MMIP-OA respectively 0.14 µm and 0.28 µm, showed a surface area for MMIP-APTES is 2874.51 m2/g and MMIP-OA 2913.07 m2/g, exhibiting superparamagnetic properties with a saturation magnetization value of MMIP-APTES 21.1 emu/g-1 and MMIP-OA 49.9 emu/g-1. Adsorption capacity result showed that MMIP-OA fits well with the Langmuir model, while MMIP-APTES fits better with the Freundlich. Application of MMIP-SPE (Magnetic Molecular Imprinted Polymer-Solid Phase Extraction) APTES resulted 92.3 ± 6.1 % and MMIP-SPE-OA 51.5 ± 8.1 % for recovering CLF in blood. The result of selectivity test also showed that MMIP-SPE-APTES is better than MMIP-SPE-OA and selectively recover CLF from human blood plasma existed together with other TB-Drugs. The study result shows that MMIPs with APTES modification can be used for CLF determination in human blood plasma.

Synthesis of molecularly imprinted polymer with a methacrylate derivative monomer for the isolation of ethyl p-methoxycinnamate as an active compound from Kaempferia galanga L. extracts.

Kaempferia galanga rhizome is traditionally used as a treatment for various diseases. Ethyl p-methoxycinnamate (EPMC), which constitutes up to 31.77% of the total essential oil, is the main/marker compound. EPMC is responsible for various pharmacological activities of Kaempferia galanga rhizome. According to the existing research, the isolation yield of EPMC is still meager, namely 0.50-2.50%; thus, a new EPMC isolation method is needed to produce better results. In this study, after determining the association constant and obtaining the Jobs plot between methacrylate derivative monomers and EPMC, a molecularly imprinted polymer for solid phase extraction (MI-SPE) was synthesized through bulk polymerization with EPMC as a template, methacrylic acid as a monomer, TRIM/EDGMA as a crosslinker in a ratio of 1 : 4 : 20 (MIP1) or 1 : 7 : 20 (MIP2). BPO was used as an initiator and n-hexane was used as a porogen. The synthesis of the NIP was also conducted using the same ratio but without the template. The MIPs were then characterized using Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) measurements, and their analytical performance was evaluated through adsorption capacity and selectivity. The results indicate that MIP2 exhibits better analytical performance with an adsorption capacity value of 0.0813 mg g-1. The selectivity of MIP2 was tested using EPMC analog compounds, namely ethyl cinnamic (EC), cinnamaldehyde (CD), and kaempferol (KF), with imprinting factor (IF) values of 17.436, 1.539, and 0.06, respectively. Lastly, MIP2 was applied to the SPE cartridge for the isolation of EPMC from Kaempferia galanga rhizome extract, and showed a percentage recovery of 82.40% for the ethanol extract, 68.05% for the ethyl acetate extract, and 65.27% for the n-hexane extract. MI-SPE 2 gives high purity results for the ethanol, ethyl acetate, and n-hexane extracts, with purities of 97.00%, 97.63%, and 99.59%, respectively. These results indicate that the MI-SPE technique shows great potential as a new method for isolating EPMCs with high yield and purity.

An indicator color chart for quick detection of Pigment Red 53 in cosmetic products in Indonesia.

BACKGROUND: Pigment Red 53 is a dangerous synthetic dye that is often added to cosmetics, even though its use in cosmetic products has been prohibited because of possible impacts on health. Faster and more sensitive detection of Pigment Red 53 is needed for onsite analysis to protect the community from illegal cosmetics that contain the dye. Indicator color charts are a kind of analytical method that can be used to detect Pigment Red 53 in cosmetic products, including lipstick, rouge, and eyeshadow. Such charts are practical, fast, and can be used for onsite analysis. METHODS: In this study, an indicator for Pigment Red 53 detection was obtained through a reagent reaction that caused a specific color change. An indicator color chart was then produced by setting out in paper form the series of colors which resulted from the reaction of specific chemical reagents and Pigment Red 53 solutions at concentrations of 10, 20, 40, 60, 80, and 100 ppm. RESULTS: The testing results showed that the indicator color chart may be used as an initial screening method for the detection of Pigment Red 53 in cosmetic products with a detectable minimum concentration of 10 ppm. Out of nine samples, only one (Eyeshadow 3) tested positive for Pigment Red 53. Further analysis was carried out on the indicator color chart and the results showed good agreement with TLC and UV-Vis spectrophotometry methods. CONCLUSION: The results reported in this paper demonstrate that the indicator color chart is a good prospective method for onsite analysis to detect Pigment Red 53 in cosmetic samples, with a lower detection limit compared to polymer-based indicators.

Separation Methods of Phenolic Compounds from Plant Extract as Antioxidant Agents Candidate.

In recent years, discovering new drug candidates has become a top priority in research. Natural products have proven to be a promising source for such discoveries as many researchers have successfully isolated bioactive compounds with various activities that show potential as drug candidates. Among these compounds, phenolic compounds have been frequently isolated due to their many biological activities, including their role as antioxidants, making them candidates for treating diseases related to oxidative stress. The isolation method is essential, and researchers have sought to find effective procedures that maximize the purity and yield of bioactive compounds. This review aims to provide information on the isolation or separation methods for phenolic compounds with antioxidant activities using column chromatography, medium-pressure liquid chromatography, high-performance liquid chromatography, counter-current chromatography, hydrophilic interaction chromatography, supercritical fluid chromatography, molecularly imprinted technologies, and high-performance thin layer chromatography. For isolation or purification, the molecularly imprinted technologies represent a more accessible and more efficient procedure because they can be applied directly to the extract to reduce the complicated isolation process. However, it still requires further development and refinement.

An Update in Computational Methods for Environmental Monitoring: Theoretical Evaluation of the Molecular and Electronic Structures of Natural Pigment-Metal Complexes.

Metals are beneficial to life, but the presence of these elements in excessive amounts can harm both organisms and the environment; therefore, detecting the presence of metals is essential. Currently, metal detection methods employ powerful instrumental techniques that require a lot of time and money. Hence, the development of efficient and effective metal indicators is essential. Several synthetic metal detectors have been made, but due to their risk of harm, the use of natural pigments is considered a potential alternative. Experiments are needed for their development, but they are expensive and time-consuming. This review explores various computational methods and approaches that can be used to investigate metal-pigment interactions because choosing the right methods and approaches will affect the reliability of the results. The results show that quantum mechanical methods (ab initio, density functional theory, and semiempirical approaches) and molecular dynamics simulations have been used. Among the available methods, the density functional theory approach with the B3LYP functional and the LANL2DZ ECP and basis set is the most promising combination due to its good accuracy and cost-effectiveness. Various experimental studies were also in good agreement with the results of computational methods. However, deeper analysis still needs to be carried out to find the best combination of functions and basis sets.