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Search results for: sample preparation techniques
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Determination of the active ingredient in pharmaceutical gel formulation by NIR spectroscopy
PublicationPharmaceuticals of their intended must be thoroughly controlled. The traditional analytical methods are very costly and time consuming. NIR spectroscopy allows to analyze pharmaceutical materials very quickly and with very low costs. First pharmaceutical applications of the NIR spectroscopy appeared with some incuriosity in the late 1960s. Application of NIR in the contemporary pharmaceutical industry is very large. The most common...
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Preparation and characterization of rigid polyurethane-polyglycerolnanocomposite foams
PublicationThis work reports on the preparation of polyurethane-polyisocyanurate (PUR-PIR) foams containing different polyglycerols and layered silicate nanoclays. The rigid polyurethane foams were obtained in a laboratory scale, in a single step method, from a two-component system with a NCO to OH groups ratio equal to two. The reaction mixture consisted of the proper amounts of a commercial oligoetherpolyol, polyglycerol, catalysts, water,...
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Blue applicability grade index (BAGI) and software: a new tool for the evaluation of method practicality
PublicationIn this work, blue applicability grade index (BAGI) is proposed as a new metric tool for evaluating the practicality of an analytical method. BAGI can be considered complementary to the well-established green metrics, and it is mainly focused on the practical aspects of White Analytical Chemistry. This tool evaluates ten main attributes including the type of analysis, the number of analytes that are simultaneously determined, the...
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Determination of organophosphorus and organonitrogen pesticides in water samples
PublicationPesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in sources of drinking water, essential to life, is a particular danger. In water, these compounds can undergo transformations, leading to the production of substances of even greater toxicity. Legal regulations are in force, stipulating the highest permissible level of...
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Speech Analytics Based on Machine Learning
PublicationIn this chapter, the process of speech data preparation for machine learning is discussed in detail. Examples of speech analytics methods applied to phonemes and allophones are shown. Further, an approach to automatic phoneme recognition involving optimized parametrization and a classifier belonging to machine learning algorithms is discussed. Feature vectors are built on the basis of descriptors coming from the music information...
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Nanoparticles preparation using microemulsion systems
PublicationMetallic nanoparticles become of current interests because they exhibit unique properties compared with those of metal atoms or bulk metal due to the quantum size effect and their large surface area, which make them attractive for applications in optics, electronics, catalysis biology and medicine. TiO2 has been used for environmental remediation purposes such as in the purification of water and air and also solar-to chemical energy...
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Properties of Nasicon-based CO2 sensor with Bi8Nb2O17 reference electrode
PublicationGas sensors are useful for the carbon dioxide concentration monitoring in many applications. The major challenge is to develop a potentiometric sensor working without the necessity of a reference gas and without a need of the reference electrode encapsulation. Important issue is a selection of reference electrode material, which should provide stable reference potential. For example as reference electrode material in sensor based...
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Synthetic Principles Determining Local Organization of Copolyesters Prepared from Lactones and Macrolactones
PublicationA highly effective and facile technique for catalytic ring-opening copolymerization (cROP) of lactones viz. ε- caprolactone and ε-decalactone with ω-pentadecalactone is being described. The reactions were mediated by Zn- and Cabased tridentate Schiff base complexes and benzyl alcohol as initiator. The catalysts were successfully employed for the preparation of numerous block and random copolymers. To unravel the composition of...
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Thin layer of ordered boron-doped TiO2 nanotubes fabricated in a novel type of electrolyte and characterized by remarkably improved photoactivity
PublicationThis paper reports a novel method of boron doped titania nanotube arrays preparation by electrochemical anodization in electrolyte containing boron precursor – boron trifluoride diethyl etherate (BF3 C4H10O), simultaneously acting as an anodizing agent. A pure, ordered TiO2 nanotubes array, as a reference sample, was also prepared in solution containing a standard etching compound: ammonium fluoride. The doped and pure titania...
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Nanoparticles: Synthesis, characteristics, and applications in analytical and other sciences
PublicationNanoparticles (NPs) are widely employed in different research areas, ranging from analytical chemistry and environmental science to medicine, the agriculture and pharmaceutical industry. This is mainly due to the unique characteristics of NPs and the novelty they introduce in such applications. In analytical chemistry, the role of NPs can differ depending on the nature of the steps involved in analytical process. NPs are probably...
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Isotope-labeled substances in analysis of persistent organicpollutants in environmental samples
PublicationUltratrace analysis of persistent organic pollutants (POPs) in environmental samples requires very sophisticated methods for both sample preparation and instrumental analysis. The complex matrix requires a multi-stage procedure. Each stage is a potential source of error, as a consequence of which the final result of analysis could be a source of misinformation rather than information. The individual stages and the procedure as...
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Methane formation over TiO2–based photocatalysts: reaction pathways
PublicationThe effects of organic impurities adsorbed or incorporated into semiconductors structure on the photocatalytic products are noteworthy. For this purpose, the as-prepared Ag, Au and Pdmodified TiO2 samples were exposed to UV-vis irradiation in various gas atmospheres (CO2, N2, 600 ppm CO2 in N2, and 13CO2) in order to clarify the route of CH4 formation in the process of photocatalytic CO2 reduction. In the presented research it...
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Elimination of excretion of ibuprofen and its metabolites in horses
PublicationAnalytical procedure based on application of gas chromatography-mass spectrometry (GC-MS) at the step of detection, identification and quantitation of ibuprofen (IBU) and detection of its metabolites – 1-hydroxyibuprofen (1-OH IBU) and carboxyibuprofen (CBX IBU) in horse urine by selected ion monitoring mode after sample preparation covering extraction at pH 3-4 and methylation has been used. The ions at m/z 161, 220 (methylated...
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Thermal degradation assessment of canola and olive oil using ultra-fast gas chromatography coupled with chemometrics
PublicationOil blending is often used to enhance the properties of vegetable oils. The admixture of a more thermally stable oil makes the resulting blend more suitable for use in frying. A new method of quality assessment of vegetable oils used in frying is presented in this paper. In this method, ultra-fast gas chromatography coupled with flame ionization detector and chemometrics is employed. Principal component analysis was used for data...
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The enantiomeric determination of chloro-precursors of methamphetamine
PublicationImpurity profiling and classification of seized methamphetamine may supply valuable information with respect to the conditions and the chemicals used in the illicit methamphetamine manufacture and may provide information on the original source of the sample. Determination of the stereochemical makeup of forensic samples is important as well for the same reasons. Laboratories in many places are engaged in clandestine manufacture...
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Liquid–phase microextraction: A review of reviews
PublicationSample preparation is an important step in chemical analysis. It is generally done to deal with problems associated with the nature of the matrix, low analyte concentrations in real samples or analyte features incompatible with the instrumentation. Classical methods of extraction consume large volumes of hazardous solvents and other reagents and are not in line with the recent emergence of green analytical chemistry. Liquid-phase...
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Toward Polyethylene–Polyester Block and Graft Copolymers with Tunable Polarity
PublicationThe synthesis and characterization of polyethylene–polyester block and graft copolymers and their potential as compatibilizers in polyethylene-based polymer blends are being described. The various routes to functionalized polyethylenes and the corresponding block/graft copolymers have been compared and evaluated for their scalability to industrial scale production. Hydroxyl chain-end and randomly OH-functionalized HDPE as well...
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Preparation and characterization of rigid polyurethane -polyglycerol nanocomposite foams
PublicationThis work reports on the preparation of polyurethane–polyisocyanurate (PUR–PIR) foams containing different polyglycerols and layered silicate nanoclays. The rigid polyurethane foams were obtained in a laboratory scale, in a single step method, from a two-component system with a NCO to OH groups ratio equal to two. The reaction mixture consisted of the proper amounts of a commercial oligoetherpolyol, polyglycerol, catalysts, water,...
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Preparation of porous TiO2 films by means of pulsed laser deposition for photocatalytic applications
PublicationIn this work the preparation and structure properties of porous thin films of TiO2 were investigated. The films were produced by means of the pulsed laser deposition technique using laser pulses at 266nm (10Hz) and at fluencies of 1-3.5J/cm2. The process was performed in vacuum using O2 buffer gas and films were deposited on the SiO2 glass or Si substrate. X-ray diffraction (XRD) and Raman analysis of the structure and chemical...
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Computational modeling of molecularly imprinted polymers as a green approach to the development of novel analytical sorbents
PublicationThe development of novel molecularly imprinted polymers (MIP) sorbents for specific chemical compounds require a lot of tedious and time-consuming laboratory work. Significant quantities of solvents and reagents are consumed in the course of the verification of appropriate configurations of polymerization reagents. Implementation of molecular modeling in the MIP sorbent development process appears to provide a solution to this...
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Rapid and simple multi-analyte LC–MS/MS method for the determination of benzodiazepines and Z-hypnotic drugs in blood samples: Development, validation and application based on three years of toxicological analyses
PublicationBenzodiazepines (BZDs) and Z-drugs have been particularly important treatments for sleeping and anxiety disorders for many years. However, recently, a number of new benzodiazepines (named designer benzodiazepines, DBZDs) were synthesised, but some of them have never been used in the clinic; they reached the black drug market as new psychoactive substances and are used for recreational purposes. The abuse of these substances has...
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Analysis of chiral pharmaceutical residues in influent and effluent samples at racemic and enantiomeric level using liquid chromatography-tandem mass spectrometry
PublicationIn this work, two different chromatographic methods for seasonal monitoring of pharmaceutical residue in wastewater samples were developed. In the case of enantiomeric separation of selected compounds, LC-MS technique combining with vancomycin based chiral stationary phase was used. The performance of chiral analysis enabled to monitor the pharmaceutical contamination at the enantiomeric level. The d-SPE procedure was developed...
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Determination of Butyltin Species in Sea Water Samples Using Solid Phase Extraction Followed by Liquid Chromatography - Tandem Mass Spectrometry
PublicationReverse phase liquid chromatography (RP-HPLC)-electrospray ionization-tandem mass spectrometry (ESI-MS-MS) was evaluated for the analysis of TBT using solid phase extraction as sample preparation method. TBT was extracted from acidified water samples (spiked with tripropyltin as internal standard) using reversed phase polymeric Strata-X cartridges. Analytes were eluted from cartridges using acetonitrile-water mixture and the volume...
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Isoprostanes-Biomarkers of Lipid Peroxidation: Their Utility in Evaluating Oxidative Stress and Analysis
PublicationIsoprostanes (IsoPs) are key biomarkers for investigating the role of free radical generation in the pathogenesis of human disorders. To solve IsoPs-related problems with regard to isoprostanes, analytical tools are required. This paper reviews the problems and trends in this field focusing on the methodology for assaying biomarkers in exhaled breath condensate (EBC) samples. A large amount of work has been done in the qualitative...
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Development of chromatographic and mass spectrometry conditions for untargeted lipidomic analysis of human breast milk
PublicationHuman breast milk (HBM) is a complex biofluid containing components which are essential for the proper growth of the newborn (for example nutrients such as carbohydrates, proteins, lipids) and also bioactive substances. According to the literature, most of studies involving HBM nutrients investigations focused essentially on the determination of proteins. The molecular composition of lipids in HBM is not well known as the protein...
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A solid phase extraction–ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples
PublicationA new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE – for sample preparation) coupled with ion chromatography–conductivity detection (IC-CD – for the final determination). Mean recoveries of...
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Deep eutectic solvents microbial toxicity: Current state of art and critical evaluation of testing methods
PublicationDeep eutectic solvents (DESs) were described at the beginning of 21st century and they consist of a mixture of two or more solid components, which gives rise to a lower melting point compared to the starting materials. Over the years, DESs have proved to be a promising alternative to traditional organic solvents and ionic liquids (ILs) due to their low volatility, low inflammability, easy preparation, and usually low cost of compounds...
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Preparation of bicyclic β-lactam and bicyclic 1,3- oxazinone scaffolds using combined cycloaddition and metathesis processes
PublicationA simple, efficient two-step method for the preparation of heterobicyclic compounds was developed. Starting from 5-acyl or 5-carbamoyl-2,2- dimethyl-1,3-dioxa-4,5-dione bicyclic scaffolds of 1-azabicyclo[5.2.0]non- 3-en-9-one, 6,9,10,10a-tetrahydro-4H-[1,3]oxazino[3,2-a]azepin-4-one, and 6,9,10,10a-tetrahydro-2H-[1,3]oxazino[3,2-a]azepine-2,4(3H)-dione were prepared using cycloaddition of thermally generated ketenes to aldimines...
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Investigations on mixture preparation for two phase adiabatic pressure drop of R134a flowing in 5 mm diameter channel
PublicationThe article presents detailed two-phase adiabatic pressure drops data for refrigerant R134a. Study cases have been set for a mass flux varying from 200 to 400 kg/m2 s, at the saturation temperature of 19.4 ◦C. Obtained experimental data was compared with the available correlations from the literature for the frictional pressure drop during adiabatic flow. Influence of mixture preparation on pressure drop was investigated, for...
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Revealing dynamic changes of the volatile profile of food samples using PTR–MS
PublicationVolatile compounds carry valuable information regarding the properties of foodstuffs. Volatiles emitted from food can be used as, for example, indicators of quality, shelf-life, or authenticity. A better understanding of the multitude of transformations which occur during food processing could facilitate the optimisation of production, increase the desirability of food products, and also their wholesomeness. However, as some of...
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Ionic liquids for nano- and microstructures preparation. Part 2: Application in synthesis
PublicationIonic liquids (ILs) are widely applied to prepare metal nanoparticles and 3D semiconductor microparticles. Generally, they serve as a structuring agent or reaction medium (solvent), however it was also demonstrated that ILs can also play a role of a co-solvent, metal precursor, reducing as well as surface modifying agent. The crucial role and possible types of interactions between ILs and growing particles have been presented in...
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Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry.
PublicationThe method for the determination of acesulfame-K, saccharine, cyclamate, aspartame, sucralose, alitame, neohesperidin dihydrochalcone, neotame and five common steviol glycosides (rebaudioside A, rebaudioside C, steviol, steviolbioside and stevioside) in soft and alcoholic beverages was developed using high-performance liquid chromatography and tandem mass spectrometry with electrospray ionisation (HPLC-ESI-MS/MS). To the best of...
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Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part I: Liquid chromatography-tandem mass spectrometry analysis
PublicationLiquid chromatography-tandem mass spectrometry with electrospray ionization (HPLC-ESI–MS/MS) methods were developed for the simultaneous determination of 42 flavouring compounds and nicotine in liquids for e-cigarettes. The chromatographic separation was performed using an Ace® Ultracore™ SuperC18™ (100 × 2.1 mm, 2.5 μm) column in both acidic and alkaline pH conditions to separate all the compounds. A simple “dilute & shoot” approach...
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SURFACTANTS IN KLODNICA RIVER (KATOWICE, POLAND). PART II. QUATERNARY AMMONIUM COMPOUNDS
PublicationThe paper presents methods of determination of analytes of the cation group (alkyl benzyl dimethyl ammonium (BDDA-C12-C16), alkyl trimethyl ammonium (TMA), hexadecyl piridinium (HP)) in surface water and bottom sediment samples. In the sample preparation phase the solid phase extraction (SPE) or accelerated solvent extraction/ultrasound assisted extraction (ASE/UAE)-SPE technique was used and in the identification phase and quantitative...
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Studies on applicability of new solid-phase microextraction fibers for the selective extraction and determination of short - chain monocarboksylic acids
PublicationShort-chain monocarobxylic acids, sometimes referred to as volatile fatty acids (VFA), are a group of low molecular weight alkyl monocarboxylic acids that are widely distributed within the environment. These molecules contain any from 2 to 8 carbon atoms and originate from the anaerobic biodegradation of organic matter such as carbohydrates, proteins, and fats. These compounds are commonly found in the effluents from animal farming,...
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Analysis of Airport Runoff Waters
PublicationA particularly important facet of airport operation is the impact of the pollution caused byrunoff waters. Runoff waters at an airport may contain relatively high concentrations of differentcontaminants resulting from the various aspects of its operation: de/anti-icing operations,washing and cleaning operations, spills of fuel and lubricants, exhaust fumes, and weed removal.The pollution caused by airport operations affects soil,...
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An evaluation of sucrose as a possible contaminant in e-liquids for electronic cigarettes by hydrophilic interaction liquid chromatography–tandem mass spectrometry
PublicationThe influence of sucrose combustion products on smoking and nicotine addiction is still controversial because the presence of the sucrose may be treated as a source of aldehydes and organic acids. In e-liquids used as refills for electronic cigarettes, which are made primarily of poly(propylene glycol), glycerine and ethanol, sucrose may be present at trace levels, and its impact on mainstream smoke formation, and hence on human...
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Quality control of cheese samples for the presence of natamycin preservative – A natural deep eutectic solvent (NADES) based extraction coupled with HPLC
PublicationA new protocol for the determination of natamycin – an antifungal agent used as a food preservative - in cheese samples – is described. This new method is based on a natural deep eutectic solvent (NADES) green extraction procedure. High-performance liquid chromatography (HPLC) was used for detection and quantification. NADESs with different molar ratios were evaluated for efficient and selective extraction. NADES made of thymol...
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Chitosan-based inks for 3D printing and bioprinting
PublicationThe advent of 3D-printing/additive manufacturing in biomedical engineering field has introduced great potential for the preparation of 3D structures that can mimic native tissues. This technology has accelerated the progress in numerous areas of regenerative medicine, especially led to a big wave of biomimetic functional scaffold developments for tissue engineering demands. In recent years, the introduction of smart bio-inks has...
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Synthesis, structural characterization, and thermal properties of Ca‐ and La‐doped soda‐lime glasses by laser melting
PublicationLaser melting techniques have been used in the preparation of unconventional glass compositions with high melting temperatures. Thus, we wanted to test the feasibility of using a CO2 laser in the preparation of nitrogen-rich oxynitride glasses and nitride silicate glasses. Melting from oxides and metallic raw materials, we wanted to study first glass formation and possible evaporation losses of the glass components. Two glass series...
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Badania połączeń spawanych rurociągu wody pitnej we Włocławku, ang. Welding joints tests in drinking water pipeline.
PublicationCelem badań opisanych w pracy było określenie przyczyn korozji powstałej w strefie wpływu ciepła (SWC) w obwodowych połączeniach spawanych w rurociągu wody pitnej. Materiałem, z którego wykonano rurociąg to stal 304/304L. W obszarze złącza spawanego stwierdzono wżery inicjowane od niezgodności geometrycznych, gdzie mogły gromadzić się osady zwiększające udział chlorków bezpośrednio przy powierzchni rury, promujące tym procesy korozyjne....
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Geographic information system for remote integration of diverse under-water acoustic sensor data
PublicationMaritime and port areas throughout the world are exposed to many different hazards, like pollution, terrorism and natural disasters. Early detection, identification and preparation of appropriateesponse strategies is especially important in the case of semi-enclosed basins like the Baltic Sea, mainly due to the marine ecosystems' continuous absorption of pollutants including oil, heavy metals and chemicals. Many of those agents...
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A Universal Gains Selection Method for Speed Observers of Induction Machine
PublicationProperties of state observers depend on proper gains selection. Each method of state estimation may require the implementation of specific techniques of finding those gains. The aim of this study is to propose a universal method of automatic gains selection and perform its verification on an induction machine speed observer. The method utilizes a genetic algorithm with fitness function which is directly based on the impulse response...
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Green Sample Collection
PublicationThe term of “green sample collection” is directly associated with both passive and dynamic analytical tools which allow for simultaneous management of the stage of collection and isolation and/or enrichment of a broad spectrum of chemical compounds from environmental samples. The use of passive sampling techniques at the stage of sample collection makes it possible to obtain in a simple yet inexpensive manner an analytical information...
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Preparation and characterization of porous scaffolds from chitosan-collagen-gelatin composite
PublicationNovel porous scaffolds composed of chitosan, collagen and gelatin were prepared and characterized. For preparing scaffolds gelatin and collagen isolated from fish skins with various physicochemical properties were used. In order to reduce preparation solubility glutaraldehyde in the amount of 1%, w/w relative to the total biopolymers weight in solution was used. All obtained biomaterials showed a homogeneous porosity. Protein polymer...
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The In-Depth Studies of Pulsed UV Laser-Modified TiO2 Nanotubes: The Influence of Geometry, Crystallinity, and Processing Parameters
PublicationThe laser processing of the titania nanotubes has been investigated in terms of morphology, structure, and optical properties of the obtained material. The length of the nanotubes and crystallinity, as well as the atmosphere of the laser treatment, were taken into account. The degree of changes of the initial geometry of nanotubes were checked by means of scanning electron microscopy, which visualizes both the surface and the cross-section....
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Lipidomics of Staphylococcus aureus – a new insight into the antibiotic resistant phenotype
PublicationStaphylococcus aureus is an aggressive pathogen responsible for a variety of diseases, in cluding life-threatening sepsis. Many strains of these bacteria are resistant to multiple classes of antibiotics, which is a substantial clinical problem in the treatment of S. aureus infections. We developed a comprehensive untargeted lipidomic workflow, including sample preparation, liquid chromatography-quadrupole-time-of-flight mass spectrometry...
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Enhanced Visible Light Active WO3 Thin Films Toward Air Purification: Effect of the Synthesis Conditions
PublicationTaking into consideration, our current environmental situation in the world people should face with growing problem of air and water pollution. Heterogeneous photocatalysis is highly promising tool to improve both, air and water quality through decomposition/mineralization of contaminations directly into harmless CO2 and H2O under ambient conditions. In this contribution we focused on the synthesis of self-assembly WO3 thin films...
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Quantum and carbon dots conjugated molecularly imprinted polymers as advanced nanomaterials for selective recognition of analytes in environmental, food and biomedical applications
PublicationSamples with complex matrix analyzed during explanation of pathogenesis of various diseases and food or environmental monitoring request advanced analytical and instrumental devices. Among the materials used for described purposes, quantum (QDs) or carbon dots (CDs) layered by molecularly imprinted polymer (MIP) shells have gained widespread attention. Unique optical and physicochemical properties of QDs/CDs together with high...
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Challenges and Possibilities of Deep Eutectic Solvent-Based Membranes
PublicationDeep eutectic solvents (DES) are a category of a new class of solvents that can overcome some of the main drawbacks of typical solvents and ionic liquids (ILs). DES have been widely investigated and applied by the research community in several applications since their invention. Over the past years, the use of DES has been directed to the production of new materials and items for new products and processes. This is the case for...