Combining mesoporous silica–magnetite and thermally-sensitive polymers for applications in hyperthermia

In this work, the synthesis strategy of a multifunctional system of [SBA-16/P(N-iPAAm)/Fe₃O₄] hybrids of interest for magneto-hyperthermia was explored. Magnetite nanoparticles coated by mesoporous silica were prepared by an alternative chemical route using neutral surfactant and without the application of any functionalization method. Monomer adsorption followed by in situ polymerization initiated by a radical was used to incorporate the hydrogel into the pore channels of the silica nanocomposite. Structural and magnetic characterization of the obtained materials was carried out by using thermal analysis, X-ray diffraction, N₂ adsorption desorption isotherms, ⁵⁷Fe Mössbauer spectroscopy, vibrating sample magnetometry and transmission electron microscopy. Measurements of alternating current magnetic-field-induced heating behaviour under different applied magnetic fields showed that the [SBA-16/P(N-iPAAm)/Fe₃O₄] hybrid here synthesized is suitable as a hyperthermia agent for biological applications.     

Developments in electrochemical processes for recycling lead–acid batteries

The lead–acid battery recycling industry is very well established, but the conventional pyrometallurgical processes are far from environmentally benign. Hence, recent developments of lead–acid battery recycling technologies have focused on low-temperature (electro)hydrometallurgical processes, the subject of this review, covering modified electrolytes, improved reaction engineering, better reactor design and control of operating conditions.     

Recent achievements on the agricultural applications of thioether derivatives: A 2010–2020 decade in review

Thioether derivatives, an important synthetic strategy in drug discovery, are acquiring more importance in plant protection field in recent years because of their broad spectrum of agricultural activities, such as antifungal, antibacterial, insecticidal, acaricidal, nematocidal, antiviral, herbicidal, and plant growth-regulating activity. Thioethers and their analogues have been an area of great interest in recent years. This review summarizes the structure and agricultural activities of the thioether derivatives as reported in the literature that mainly covers the past 10 years from 2010 to 2020 as well as may contribute to a better understanding of thioether derivatives as efficient agricultural agents and provide some ideas on the development of novel pesticides.     

Capillary electrophoresis-mass spectrometry for intact protein analysis: Pharmaceutical and biomedical applications (2018–March 2023)

Capillary electrophoresis is recognized as a valued separation technique for its high separation efficiency, low sample consumption, good economic and ecological aspects, reproducibility, and complementarity to traditional liquid chromatography techniques. Capillary electrophoresis experiments are generally performed utilizing optical detection, such as ultraviolet or fluorescence detectors. However, in order to provide structural information, capillary electrophoresis hyphenated to highly sensitive and selective mass spectrometry has been developed to overcome the limitations of optical detections. Capillary electrophoresis-mass spectrometry is increasingly popular in protein analysis, including biopharmaceutical and biomedical research. It is frequently applied for the determination of physicochemical and biochemical parameters of proteins, offers excellent performance for in-depth characterizations of biopharmaceuticals at various levels of analysis, and has been also already proven as a promising tool in biomarker discovery. In this review, we focus on the possibilities and limitations of capillary electrophoresis-mass spectrometry for protein analysis at their intact level. Various capillary electrophoresis modes and capillary electrophoresis-mass spectrometry interfaces, as well as approaches to prevent protein adsorption and to enhance sample loading capacity, are discussed and the recent (2018–March 2023) developments and applications in the field of biopharmaceutical and biomedical analysis are summarized.     

Current trends and challenges in sample preparation for global metabolomics using liquid chromatography–mass spectrometry

The choice of sample-preparation method is extremely important in metabolomic studies because it affects both the observed metabolite content and biological interpretation of the data. An ideal sample-preparation method for global metabolomics should (i) be as non-selective as possible to ensure adequate depth of metabolite coverage; (ii) be simple and fast to prevent metabolite loss and/or degradation during the preparation procedure and enable high-throughput; (iii) be reproducible; and (iv) incorporate a metabolism-quenching step to represent true metabolome composition at the time of sampling. Despite its importance, sample preparation is often an overlooked aspect of metabolomics, so the focus of this review is to explore the role, challenges, and trends in sample preparation specifically within the context of global metabolomics by liquid chromatography-mass spectrometry (LC-MS). This review will cover the most common methods including solvent precipitation and extraction, solid-phase extraction and ultrafiltration, and discuss how to improve analytical quality and metabolite coverage in metabolomic studies of biofluids, tissues, and mammalian cells. Recent developments in this field will also be critically examined, including in vivo methods, turbulent-flow chromatography, and dried blood spot sampling.     

Recent developments and applications of capillary and microchip electrophoresis in proteomics and peptidomics (mid-2018–2022)

This review gives a wide overview of recent advances and applications of capillary electrophoresis and microchip capillary electrophoresis methods in the fields of proteomics and peptidomics in the period from mid-2018 up to the end of 2022. The methodological topics covering sample preparation and concentration techniques, hyphenation of capillary electrophoresis methods with mass spectrometry, and multidimensional separations by on-line or off-line coupled different capillary electrophoresis and liquid chromatography techniques are described and new developments in both bottom-up and top-down approaches in proteomics are presented. In addition, various applications of capillary electrophoresis methods in proteomic and peptidomic studies are demonstrated. They include monitoring of protein posttranslational modifications and applications in biological and biochemical research, clinical peptidomics and proteomics, and food analysis.     

Ambient air temperature and degree-day data analysis of the period 2006–2017 for Cyprus

Journal of Thermal Analysis and Calorimetry - Heating degree days (HDDs) and cooling degree days (CDDs) are widespread climatic indicators that depict the extremity and duration of ambient air...     

Tritium in surface waters, tap water and in precipitation in Poland during the 1994–1999 period

Concentrations of tritium in environmental waters (precipitation, rivers, lakes, tap water) have been determined using electrolytic enrichment and liquid scintillation counting. In waters of big rivers (the Vistula and the Odra rivers), lakes and tap water the annual average concentrations were similar to each other being from 1.4 to 1.9 Bq·dm^-3. These concentrations were similar to those in the precipitation in which they ranged from 1.7 to 2.2 Bq·dm^-3. The lowest tritium concentrations were found in waters of the Seashore Region rivers (average for 1994–1999 was 1.1 Bq·dm^-3). The tritium concentrations in surface waters and in precipitation are still higher than that of natural level. The data obtained show that tritium concentration in the water of rivers might depend on the size of drainage area. The observed seasonal variations of tritium concentration in the precipitation collected in Warsaw and at the Mount Sniezka indicate the stratospheric source of tritium. It was found that about 30% of tritium deposited with precipitation is removed to the Baltic Sea with river waters.     

Microgel,nanogel and hydrogel–hydrogel semi-IPN composites for biomedical applications: synthesis and characterization

Quaternary ammonium salt hydrogels from a cationic monomer, (3-acrylamidopropyl)-trimethylammonium chloride (APTMACl), in a variety sizes such as bulk, micro- and nano- has been prepared. The synthesis of micro- and nanogels were carried out in the microenvironment of water-in-oil microemulsions using two types of surfactants, namely, L-α- phosphatidylcholine (lecithin) and dioctyl sulfosuccinate sodium salt (AOT). Additionally, hydrogel–hydrogel composite semi-interpenetrating polymer networks (semi-IPN) was synthesized by dispersing previously prepared micro/nanogel into neutral monomers such as acrylamide (AAm) or 2-hydroxylethyl methcarylate (HEMA) before network formation. Hydrogel swelling and pH response behaviors have been investigated for bulk gels. Morphology, structure, and size of nano-, micro- and bulk materials were explored utilizing transmission electron microcopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM). It was confirmed with gel electrophoresis that completely charged nanogel form a strong complex with DNA.     

Synthetic applications of rongalite: A green tool in the service of Diels–Alder chemistry and beyond

Rongalite or sodium hydroxymethanesulfinate dihydrate acts as a bleaching agent and it is used in printing and dying industry. Due to its ability to deliver SO₂ dianion, rongalite is useful to prepare sultines and sulfones. We have been exploiting its potential towards the construction of diverse polycylic frameworks. This account describes the utility of rongalite to expand the Diels–Alder chemistry via sultine or sulfone derivatives. In this context, rongalite played a critical role to increase the chemical space of unnatural amino acids, spirocycles, polycycles, sulfones and crown ethers.     

Comparison of four types of gamma- and X-ray detectors for environmental applications in the 10–450 keV energy range

The performance of four types of - and X-ray radiation detectors for environmental applications was evaluated in the 10–450 keV energy range. Two cadmium zinc telluride (CdZnTe) room temperature semiconductor detectors were evaluated along with a cryogenically cooled semiconductor detector and two different types of scintillation detectors. The energy resolution, absolute peak detection efficiency and peak-to-background ratio of each of the detectors were calculated and intercompared. The advantages and disadvantages of environmental applications of each detector, along with their performance results, are summarized.     

Ionic liquid–solid interface and applications in lubrication and energy storage

Room-temperature ionic liquids (ILs) exhibit many attractive properties in proximity to solid surfaces. Primarily, they form well-defined interfacial layers that are tunable — electrically and thermally — as well as being stable — mechanically, electrically, and thermally — over a wide range. Recent investigations have aimed at understanding the molecular structuring of ILs at their interface with solids and in confinement, while in tandem, ILs are used as next-generation lubricants and energy storage materials. The result is a large volume of work that has appeared over the last decade. In this review, the recent literature is presented and future research directions are discussed.     

Developments in ion mobility spectrometry–mass spectrometry

Ion mobility spectrometry (IMS) has been used for over 30 years as a sensitive detector of organic compounds. The following is a brief review of IMS and its principles with an emphasis on its usage when coupled to mass spectrometry. Since its inception, IMS has been interfaced with quadrupole, time-of-flight, and Fourier-transform ion cyclotron resonance mass spectrometry. These hybrid instruments have been employed for the analysis of a variety of target analytes, including biomolecules, explosives, chemical warfare degradation products, and illicit drugs.     

Electron beam accelerators—trends in radiation processing technology for industrial and environmental applications in Latin America and the Caribbean

The radiation processing technology for industrial and environmental applications has been developed and used worldwide. In Latin America and the Caribbean and particularly in Brazil there are 24 and 16 industrial electron beam accelerators (EBA) respectively with energy from 200 keV to 10 MeV, operating in private companies and governmental institutions to enhance the physical and chemical properties of materials. However, there are more than 1500 high-current electron beam accelerators in commercial use throughout the world. The major needs and end-use markets for these electron beam (EB) units are R and D, wire and electric cables, heat shrinkable tubes and films, PE foams, tires, components, semiconductors and multilayer packaging films. Nowadays, the emerging opportunities in Latin America and the Caribbean are paints, adhesives and coatings cure in order to eliminate VOCs and for less energy use than thermal process; disinfestations of seeds; and films and multilayer packaging irradiation. For low-energy EBA (from 150 keV to 300 keV). For mid-energy EBA (from 300 keV to 5 MeV), they are flue gas treatment (SO₂ and NO_X removal); composite and nanocomposite materials; biodegradable composites based on biorenewable resources; human tissue sterilization; carbon and silicon carbide fibers irradiation; irradiated grafting ion-exchange membranes for fuel cells application; electrocatalysts nanoparticles production; and natural polymers irradiation and biodegradable blends production. For high-energy EBA (from 5 MeV to 10 MeV), they are sterilization of medical, pharmaceutical and biological products; gemstone enhancement; treatment of industrial and domestic effluents and sludge; preservation and disinfestations of foods and agricultural products; soil disinfestations; lignocellulosic material irradiation as a pretreatment to produce ethanol biofuel; decontamination of pesticide packing; solid residues remediation; organic compounds removal from wastewater; and treatment of effluent from petroleum production units and liquid irradiation process to treat vessel water ballast. On the other hand, there is a growing need of mobile EB facilities for different applications in South America.     

Development and validation of HPLC method for the determination of α-tocopherol in human erythrocytes for clinical applications

In this work, a simple isocratic reversed-phase HPLC method for determination of alpha-tocopherol in human erythrocytes has been developed and validated. After separation of plasma the erythrocytes were washed three times with 0.9% sodium chloride containing 0.01% butylated hydroxytoluene (BHT) as antioxidant and then were diluted 1:1 (v/v) with the same solution. In the liquid-liquid extraction (LLE) procedure, 2500 microL of n-hexane was added to 500 microL of erythrocytes. After 2 min this mixture was deproteinized by addition of cool ethanol (500 microL, 5 min) denatured with 5% methanol containing alpha-tocopherol acetate (20 micromol L(-1)), as internal standard, and then extracted for 5 min by vortex mixing. After centrifugation (10 min, 1600xg) an aliquot (2000 microL) of the clean extract was separated and evaporated under nitrogen. The residue was dissolved in 400 microL methanol and analysed by reversed-phase HPLC on a 4.6 mmx150 mm, 5 microm Pecosphere C18 column; the mobile phase was 100% methanol, flow rate 1.2 mL min(-1). The volume injected was 100 microL and detection was by diode-array detector at a wavelength of 295 nm. The extraction recovery of alpha-tocopherol from human erythrocytes was 100.0+/-2.0%. The detection limit was 0.1 micromol L(-1) and a linear calibration plot was obtained in the concentration range 0.5-20.0 micromol L(-1). Within determination precision was 5.2% RSD (n=10), between determination precision was 6.1% RSD (n=10). The method was applied successfully in a clinical study of patients with acute pancreatitis and for determination of the reference values in the healthy Czech population.     

Developments in the synthesis of α,α-dibromoacetophenones and related compounds

Increasing demand of α,α-dibromoketones, as highly reactive and easy-to-handle precursors to carry out selective organic transformations, to synthesize heterocyclic compounds of therapeutic interest and lack of any compilation on this subject prompted us to assemble the methods available for their synthesis.     

Customization of the CEFM for predicting stress corrosion cracking in lightly sensitized Al–Mg alloys in marine applications

The Coupled Environment Fracture Model (CEFM) has been modified and calibrated to predict crack growth rate (CGR) in aluminum marine alloys. The customized CEFM provided quantitative predictions of the effects of O₂, electrochemical potential, stress intensity factor, and conductivity on CGR in lightly sensitized AA5083-H321 in 3.5 wt.% NaCl solution, as well as explaining the development of a semi-elliptical surface cracks. The importance of the properties of the external environment, such as conductivity, oxidant/reductant concentration, and the kinetics of the cathodic reactions on the surfaces external to the crack has been confirmed. Crack growth is attributed to a sequence of microfracture events at the crack front, the frequency of which is determined by the mechanical conditions that exist at the crack tip, as governed by the stress intensity while the microfracture dimension is determined by hydrogen-induced fracture, with the CGR being the product of these two quantities. The success in explaining the intergranular stress corrosion cracking (IGSCC) of aluminum alloys, argues that the basic concept of the CEFM, that the internal and external environments are strongly coupled, is sound and that the CEFM, which was originally developed to describe IGSCC in sensitized stainless steels is equally applicable for describing IGSCC in lightly sensitized aluminum alloys.