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Dalton Transactions (Cambridge, England... Nov 2023An organic cation lacking specificity in its structure-directing action offers the possibility, through the screening of other structure-directing parameters, to...
An organic cation lacking specificity in its structure-directing action offers the possibility, through the screening of other structure-directing parameters, to synthesize a variety of zeolites. In this work we show that the organic structure-directing agent 2-isopropyl-1,3-dimethylimidazolium (2iPr13DMI) can produce up to seven different zeolite phases depending on water concentration, the presence of inorganic impurities, crystallization temperature and time, and germanium molar fraction. The obtained phases are very different in terms of pore system, connectivity of the zeolite structure and structural units. At the pure SiO side, ZSM-12 and SSZ-35 dominate, with ZSM-12 being favored by the presence of potassium impurities and by less concentrated conditions. The introduction of Ge at low levels favors SSZ-35 over ZSM-12 and as the Ge fraction increases it successively affords CSV, -CLO and two distinct UOS zeolites, HPM-11 and HPM-6. These two zeolites have the same topology but distinct chemical compositions and display powder X-ray diffraction patterns that are much different from each other and from that of as-synthesized IM-16 (UOS reference material). They also show different symmetry at 96 K. Rietveld refinements of the three as-made UOS materials mentioned are provided. HPM-6 and HPM-11 are produced in distinct, non-adjacent crystallization fields. The frequent cocrystallization of the chiral STW zeolite, however, did not afford its synthesis as a pure phase. Molecular mechanics simulations of the location of the organic cation and host-guest interactions fail to explain the observed trends, but also considering the intrinsic stability of the zeolites and the effect of germanium help to rationalize the results. The study is completed by DFT calculations of the NMR chemical shifts of C in UOS (helping to understand splittings in the spectrum) and F in CSV (supporting the location of fluoride inside the new [45], which is an incomplete double 4-ring).
PubMed: 37791957
DOI: 10.1039/d3dt02414h -
Polymers Aug 2023The safety of a medicinal product is determined by its pharmacological and toxicological profile, which depends not only on the active substance's toxicological... (Review)
Review
The safety of a medicinal product is determined by its pharmacological and toxicological profile, which depends not only on the active substance's toxicological properties, but also on the impurities it contains. Because impurities are a problem that must be considered to ensure the safety of a drug product, many studies have been conducted regarding the separation or purification of active pharmaceutical ingredients (APIs) and the determination of impurities in APIs and drug products. Several studies have applied molecularly imprinted polymers (MIPs) to separate impurities in active ingredients and as adsorbents in the sample preparation process. This review presents the design of MIPs and the methods used to synthesise MIPs to separate impurities in APIs and drug product samples, the application of MIPs to separate impurities, and a view of future studies involving MIPs to remove impurities from pharmaceutical products. Based on a comparison of the bulk and surface-imprinting polymerisation methods, the MIPs produced by the surface-imprinting polymerisation method have a higher adsorption capacity and faster adsorption kinetics than the MIPs produced by the bulk polymerisation method. However, the application of MIPs in the analysis of APIs and drug products are currently only related to organic compounds. Considering the advantages of MIPs to separate impurities, MIPs for other impurities still need to be developed, including multi-template MIPs for simultaneous separation of multiple impurities.
PubMed: 37631457
DOI: 10.3390/polym15163401 -
The Science of the Total Environment Oct 2022A 620-day batch experiment was conducted to examine the generation of nano-sized plastic particles and migration of organic compounds derived from plastic additives and...
A 620-day batch experiment was conducted to examine the generation of nano-sized plastic particles and migration of organic compounds derived from plastic additives and impurities during the weathering of three common plastic types in water with and without reactive oxygen species. The results show that the amount of nanoplastics plus organic compounds liberated from the tested plastic films, as indicated by total organic carbon, was in the following decreasing order: PET >PP > ABS. Hydroxyl radical generated from Fenton-like reaction significantly enhanced the generation of nanoplastics and release of organic compounds from the weathered plastic films via oxidative degradation. Over 30 organic compounds including potentially toxic organic pollutants originated from plastic additives and impurities were detected. There was a marked difference in the plastic nanoparticle size distribution between the deionized water and the water containing reactive oxygen species. The strong oxidizing capacity of hydroxyl radical resulted in rapider disintegration of the coarser nanoparticles (>500 nm) into the finer nanoparticles (<500 nm) and allowed complete decomposition of the nanoplastics with a size <50 nm or even <100 nm. Elevated level of Ca was detected on the surfaces of the ABS and PP nanoparticles. PP- and PET-derived nanoplastics contained heavy metal(loid)s while no heavy metal(loid)s was detected for the ABS nanoparticles. PET nanoparticles had a stronger capacity to bind S- and N-containing organic ligands compared to the other two plastic nanoparticles. The nanoplastics generated from the weathering were irregular in shape, which means that they had larger specific area compared to spherical engineered nanoplastics.
Topics: Hydroxyl Radical; Microplastics; Nanoparticles; Organic Chemicals; Plastics; Reactive Oxygen Species; Water; Water Pollutants, Chemical
PubMed: 35750181
DOI: 10.1016/j.scitotenv.2022.156859 -
Biophysical Reviews Oct 2023In today's world, there is a wide array of materials engineered at the nano- and microscale, with numerous applications attributed to these innovations. This review aims... (Review)
Review
In today's world, there is a wide array of materials engineered at the nano- and microscale, with numerous applications attributed to these innovations. This review aims to provide a concise overview of how nano- and micromaterials are utilized for enzyme immobilization. Enzymes act as eco-friendly biocatalysts extensively used in various industries and medicine. However, their widespread adoption faces challenges due to factors such as enzyme instability under different conditions, resulting in reduced effectiveness, high costs, and limited reusability. To address these issues, researchers have explored immobilization techniques using nano- and microscale materials as a potential solution. Such techniques offer the promise of enhancing enzyme stability against varying temperatures, solvents, pH levels, pollutants, and impurities. Consequently, enzyme immobilization remains a subject of great interest within both the scientific community and the industrial sector. As of now, the primary goal of enzyme immobilization is not solely limited to enabling reusability and stability. It has been demonstrated as a powerful tool to enhance various enzyme properties and improve biocatalyst performance and characteristics. The integration of nano- and microscale materials into biomedical devices is seamless, given the similarity in size to most biological systems. Common materials employed in developing these nanotechnology products include synthetic polymers, carbon-based nanomaterials, magnetic micro- and nanoparticles, metal and metal oxide nanoparticles, metal-organic frameworks, nano-sized mesoporous hydrogen-bonded organic frameworks, protein-based nano-delivery systems, lipid-based nano- and micromaterials, and polysaccharide-based nanoparticles.
PubMed: 37975005
DOI: 10.1007/s12551-023-01146-6 -
Water Science and Technology : a... Nov 2022Due to industrialization and population growth, freshwater supplies are diminishing and becoming impure with high organic pollutant concentrations such as nitrate and... (Review)
Review
Due to industrialization and population growth, freshwater supplies are diminishing and becoming impure with high organic pollutant concentrations such as nitrate and phosphate, which shows a high adverse impact on aquatic and human lives. In drinking water sources, particularly groundwater, nitrate is considered as one of the major pollutants which causes methemoglobinemia (in newborn infants), carcinogenic activities and diabetes. Excess concentration of phosphate leads to eutrophication and death of aquatic species due to reduced dissolved oxygen content. Therefore, all countries must implement highly effective technologies for treating wastewater. Chitosan and zeolite are naturally occurring and cost-effective adsorbent materials with a higher surface area that exhibit greater nitrate and phosphate adsorption. Surface modification of chitosan and zeolite increases the adsorption capacity of adsorbents for the removal of both anions selectively. This paper reviews the current development of modified chitosan and zeolite adsorbents for anion adsorption, with an emphasis on modification by zero and multivalent metals and metal oxides, different surfactants, biomass-derived carbon, and natural and synthetic polymers. Multiple adsorption parameters, optimum adsorption condition, adsorption mechanism, regeneration study, research gap and future aspects have been explained for further research work.
Topics: Infant; Infant, Newborn; Humans; Nitrates; Phosphates; Zeolites; Chitosan; Nitrogen Oxides; Environmental Pollutants
PubMed: 36450679
DOI: 10.2166/wst.2022.366 -
Waste Management (New York, N.Y.) Mar 2022Digestate is a nutrient-rich by-product from organic waste anaerobic digestion but can contribute to nutrient pollution without comprehensive management strategies. Some... (Review)
Review
Digestate is a nutrient-rich by-product from organic waste anaerobic digestion but can contribute to nutrient pollution without comprehensive management strategies. Some nutrient pollution impacts include harmful algal blooms, hypoxia, and eutrophication. This contribution explores current productive uses of digestate by analyzing its feedstocks, processing technologies, economics, product quality, impurities, incentive policies, and regulations. The analyzed studies found that feedstock, processing technology, and process operating conditions highly influence the digestate product characteristics. Also, incentive policies and regulations for managing organic waste by anaerobic digestion and producing digestate as a valuable product promote economic benefits. However, there are not many governmental and industry-led quality assurance certification systems for supporting commercializing digestate products. The sustainable and safe use of digestate in different applications needs further development of technologies and processes. Also, incentives for digestate use, quality regulation, and social awareness are essential to promote digestate product commercialization as part of the organic waste circular economy paradigm. Therefore, future studies about circular business models and standardized international regulations for digestate products are needed.
Topics: Anaerobiosis; Environment; Eutrophication
PubMed: 35032793
DOI: 10.1016/j.wasman.2021.12.035 -
Biomass Conversion and Biorefinery Mar 2023Crude glycerol (CG) and glycerol pitch (GP) are highly alkaline residues from biodiesel and oleochemical plants, respectively, and have organic content which incurs high...
UNLABELLED
Crude glycerol (CG) and glycerol pitch (GP) are highly alkaline residues from biodiesel and oleochemical plants, respectively, and have organic content which incurs high disposal cost and poses an environmental threat. Characterization of these residues for composition and properties could provide insight into their quality for proper disposal and can help the biodiesel industry to adopt more sustainable practices, such as reducing waste and improving the efficiency of the production process, hence minimizing the impact of the biodiesel supply chain to the environment. These data also allow the identification and exploration of new ways for their utilization and transformation into highly value-added products. In this study, we evaluated four CG samples (B, C, D, and E) and two GP samples (F and G) obtained from Malaysian palm oil refineries, and the results were compared with pure glycerol (A). Spectroscopic analysis was performed using FTIR, H-, and C-NMR. All samples had similar density to A (1.26 g/cm), except for F (1.31 g/cm), while the density for E and G could not be determined due to their physical states. The pH and viscosity largely varied in the range of 7.26-11.89 and 43-225 cSt, respectively. The glycerol content of CG (B, C, D, and E) was high and consistent (81.7-87.3%) whereas GP F and G had 71.5 and 63.9% glycerol content, respectively. Major contaminants in CG and GP were water and matter organic non-glycerol (MONG), respectively. The water, ash, soap, and salt content were considerably low, which varied from 3.4 to 14.1%, 3.9 to 13.0%, 0.1 to 5.7%, and 4.1 to 9.2% respectively. Thermal analysis of CG and GP exhibited four phases of decomposition attributed to the impurities compared to the single phase in A. All samples had calorific values lower than A (18.1 MJ/kg) between 9.0 and 17.7 MJ/kg. Based on the results, CG and GP have high glycerol content which reveals their potential to be used as feedstock in bioconversion and chemical or thermal treatment while impurities may be removed by pre-treatment if required. As palm oil is one of the main feedstocks for the oleochemical industry, this work underlines the importance of characterization of the residue generated to provide additional data and information on palm-based agricultural industry wastes, minimize the impact of palm oil supply chain on the environment, and explore its potential usage for value-addition.
SUPPLEMENTARY INFORMATION
The online version contains supplementary material available at 10.1007/s13399-023-04003-4.
PubMed: 37363204
DOI: 10.1007/s13399-023-04003-4 -
Biomedical Chromatography : BMC Apr 2022Montelukast sodium (MLS) is a leukotriene receptor antagonist drug used in the treatment of asthma, bronchospasm, allergic rhinitis and urticaria. A reversed-phase high...
Montelukast sodium (MLS) is a leukotriene receptor antagonist drug used in the treatment of asthma, bronchospasm, allergic rhinitis and urticaria. A reversed-phase high performance liquid chromatography method was developed to separate, identify and quantitative determination of MLS and its eight known organic impurities in tablet dosage form using a C column and mobile phases consisting of a gradient mixture of pH 2.5 phosphate buffer and acetonitrile. The stability-indicating character of the developed method was proven using stress testing (1 m HCl at 80°C/30 min, 1 m NaOH at 80°C/30 min, H O at 80°C/30 min, 3% H O at 25°C/1 min, dry heat at 105°C/10 h and UV-vis light/4 days) and was validated for specificity, quantitation limit, linearity, precision, accuracy and robustness. For MLS and its eight known impurities, the quantitation limits, linearity and recoveries were 0.015-0.03 μg/ml, correlation coefficient > 0.997 (R > 0.995) and 85.5-107.0%, respectively. The developed chromatographic method is suitable for impurity profiling and also for assay determination of MLS in bulk drugs and pharmaceutical formulations. The mass values (m/z) of newly formed degradation products (DP1 and DP2) of montelukast sodium were identified using liquid chromatography-mass spectrometry.
Topics: Acetates; Chromatography, High Pressure Liquid; Chromatography, Liquid; Cyclopropanes; Drug Stability; Quinolines; Reproducibility of Results; Sulfides; Tablets
PubMed: 34994006
DOI: 10.1002/bmc.5330 -
Biomedical Chromatography : BMC Jun 2023The aim of this study is to develop a stability-indicating, reversed-phase HPLC method for the quantification of assay and organic impurities (process and degradation)...
The aim of this study is to develop a stability-indicating, reversed-phase HPLC method for the quantification of assay and organic impurities (process and degradation) of doxycycline hyclate in a doxycycline injectable formulation. Both the active and dosage forms are officially present in the USP monograph, and assay and impurity methods are provided by separate UPLC techniques, which are highly sensitive to the flow rate and temperature, considering the quality control requirements and user-friendliness. A simple stability-indicating HPLC method with a shorter run time was developed for the simultaneous quantification of assay and impurity. The method was developed using HPLC with a gradient program and a reversed-phase Waters XBridge BEH C8 column (150 × 4.6 mm, 3.5 μm i.d.). Mobile phase A consisted of phosphate buffer (pH 8.5, 25 mM potassium phosphate, 2 mM ethylenediaminetetraacetic acid, and 0.5 ml of triethylamine). Mobile phase B consisted of methanol with a flow rate of 1.7 ml/min, a column temperature of 55°C, a UV wavelength of 270 nm, and an injection volume of 25 μl. Modern research represents a concomitant method for quantifying assay and organic impurities of doxycycline hyclate (active form) and doxycycline for injection (dosage form). The assay and impurity method were validated per United States Pharmacopeia (USP) 1225 and International Conference on Harmonization (ICH) guidelines. The retention time of doxycycline and degradation impurity, 4-epidoxycycline, was about 9.8 and 6.4 min, respectively. The linearity range of doxycycline and 4-epidoxycycline was 0.5-150 and 0.5-18 μg/ml, respectively. The percentage of recovery of doxycycline and 4-epidoxycycline was 98.7-100.6% and 88.0-112.0%. Validation of the analytical method demonstrated that the method is suitable, specific, linear, accurate, precise, rugged, and stability indicating for estimating the assay, known and degraded impurities of doxycycline, and doxycycline for injection.
Topics: Chromatography, High Pressure Liquid; Drug Stability; Doxycycline; Quality Control
PubMed: 36930874
DOI: 10.1002/bmc.5626 -
Advanced Materials (Deerfield Beach,... May 2020Organophosphorus (OP)-based nerve agents are extremely toxic and potent acetylcholinesterase inhibitors and recent attacks involving nerve agents highlight the need for... (Review)
Review
Organophosphorus (OP)-based nerve agents are extremely toxic and potent acetylcholinesterase inhibitors and recent attacks involving nerve agents highlight the need for fast detection and intervention. Fluorescence-based detection, where the sensing material undergoes a chemical reaction with the agent causing a measurable change in the luminescence, is one method for sensing and identifying nerve agents. Most studies use the simulants diethylchlorophosphate and di-iso-propylfluorophosphate to evaluate the performance of sensors due to their reduced toxicity relative to OP nerve agents. While detection of nerve agent simulants in solution is relatively widely reported, there are fewer reports on vapor detection using solid-state sensors. Herein, progress in organic semiconductor sensing materials developed for solid-state detection of OP-based nerve agent vapors is reviewed. The effect of acid impurities arising from the hydrolysis of simulants and nerve agents on the efficacy and selectivity of the reported sensing materials is also discussed. Indeed, in some cases it is unclear whether it is the simulant that is detected or the acid hydrolysis products. Finally, it is highlighted that while analyte diffusion into the sensing film is critical in the design of fast, responsive sensing systems, it is an area that is currently not well studied.
Topics: Chemical Warfare Agents; False Positive Reactions; Spectrometry, Fluorescence; Volatilization
PubMed: 31692155
DOI: 10.1002/adma.201905785