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Wyniki wyszukiwania dla: organometallic chemistry
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Intramolecular interactions in crystals of tris(2,6-diisopropylphenoxy)silanethiol and its sodium salts
PublikacjaHydrolytically stable tris(2,6-diisopropylphenoxy)silanethiol has been obtained and reacted with sodium. Solid state interactions within and between the molecules of tris(2,6-diisopropylphenoxy)silanethiol including S-H---π-interactions between the S-H unit and the π-system of the arene have been analyzed. The interactions are documented by X-ray diffraction and FT-IR spectroscopy.
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Chiral analysis of chloro intermediates of methylamphetamine by one-dimensional and multidementional NMR and GC/MS
PublikacjaImpurity profiling and classification of abused drugs using chiral analytical techniques is of particular interest and importance because of the additional information obtained fromthis approach. When these methods are applied to the synthesis of illicitly used substances, they can supply valuable information about the conditions/chemicals used in the synthesis. We have applied GC and NMR methods to the study of intermediates found...
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Chromogenic amides of pyridine-2,6-dicarboxylic acid as anion receptors
PublikacjaThe synthesis of simple, chromogenic pyridine-2,6-dicarboxylic acid amides, derivates of isomeric nitroanilines and aminonitrophenols, and their ion binding properties are described. The ligands' response to ionic species was examined by naked eye and was studied with the use of UV-Vis spectroscopy in DMSO and its mixture with water. The effect of the localisation and the type of the substituents in aromatic rings were discussed....
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Selective detection of F- by chromogenic tetrazole receptor
PublikacjaA chromogenic anion host 4, containing two amide functionalities linked to azo dye and tetrazole rings was synthesized and its complexes with various anions were investigated. The results show that receptor 4 can recognize selectively biologically important F- ion. The binding affinity for F- was investigated by naked-eye colour change, UV-Vis and 1H NMR spectroscopy. Addition F- ion in CH3CN and DMSO to receptor 4 cause a colour...
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Reactions of Lithiated Diphosphanes R2P−P(SiMe3)Li (R = tBu and iPr) with [MeNacnacTiCl2·THF] and [MeNacnacTiCl3]. Formation and Structure of TitaniumIII and TitaniumIV β‑Diketiminato Complexes Bearing the Side-on Phosphanylphosphido and Phosphanylphosphinidene Functionalities
Publikacjaβ-Diketiminate complexes of TiIII-containing phosphanylphosphido ligands [MeNacnacTi(Cl){η2-P(SiMe3)- PR2}] (MeNacnac− = [Ar]NC(Me)CHC(Me)N[Ar]; Ar = 2,6- iPr2C6H3) were prepared by reactions of [MeNacnacTiCl2· THF] with lithium derivatives of diphosphanes R2P−P(SiMe3) Li (R = tBu, iPr) in toluene solutions. Surprisingly, reactions of [MeNacnacTiCl2·THF] with R2P−P(SiMe3)Li in THF solutions led to TiIV complexes containing phosphanylphosphinidene ligands...
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Geometry optimization of steroid sulfatase inhibitors - the influence on the free binding energy with STS
PublikacjaIn the paper we review the application of two techniques (molecular mechanics and quantum mechanics) to study the influence of geometry optimization of the steroid sulfatase inhibitors on the values of descriptors coded their chemical structure and their free binding energy with the STS protein. We selected 22 STS-inhibitors and compared their structures optimized with MM+, PM7 and DFT B3LYP/6–31++G* approaches considering separately...
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FT-Raman spectroscopy as a tool in evaluation the response of plants to drought stress
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Application of a magnetically separable Zr-MOF for fast extraction of palladium before its spectrophotometric detection
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Sandwich-type architecture film based on WS2 and ultrafast self-expanded and reduced graphene oxide in a Li-ion battery
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The effect of manganese on the structural and surface properties of nanocrystalline cobalt catalyst for ammonia synthesis
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Kinetics of aquation of [Co(ODA)(H2O)3] induced by Fe(III)
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Investigations of ternary complexes of Co(II) and Ni(II) with oxydiacetate anion and 1,10-phenanthroline or 2,2′-bipyridine in solutions
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Application of a novel deep eutectic solvent modified carbon nanotube for pipette-tip micro solid phase extraction of 6-mercaptopurine
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Bonding interactions in oxydiacetate and thiodiacetate cobalt(II) and nickel(II) complexes
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Investigations of ternary complexes of Co(II) and Ni(II) with thiodiacetate anion and 1,10-phenanthroline or 2,2’-bipyridine in aqueous solutions
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The effect of aluminium oxide on the reduction of cobalt oxide and thermostabillity of cobalt and cobalt oxide
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Response of murine gut microbiota to a prebiotic based on oligosaccharides derived via hydrolysis of fungal α-(1→3)-d-glucan: Preclinical trial study on mice
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Studies on selectivity of hydrocarbon group type separation of petroleum vacuum distillates and base oils by HPLC.
PublikacjaW pracy przedstawiono wyniki badań nad doborem selektywnego chromatograficznego układu HPLC, umożliwiającego rozdzielenie grupowe produktów naftowych otrzymanych z destylacji próżniowej ropy naftowej, w tym, mineralnych olejów bazowych. Stwierdzono, że konieczny układ chromatograficzny wymaga wykorzystania dwóch kolumn wypełnionych żelem krzemionkowym ze związanymi grupami nitrofenopropylowymi, połączonych szeregowo z dwiema...
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Calibration of permeation passive samplers with silicone membranes based on physicochemical properties of the analytes.
PublikacjaW pracy opisano sposób kalibracji pasywnych dozymetrów permeacyjnych, wykorzystywanych w badaniach powietrza w oparciu o własności fizyko-chemiczne analitów. Stwierdzono silną zależność pomiędzy stałą kalibracyjną (K) dozymetrów i liczbą atomów węgla w cząsteczce analitu (w obrębie danej grupy związków chemicznych) dla alkoholi, alifatycznych i aromatycznych węglowodorów oraz estrów. Taka zależność występuje również pomiędzy...
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Reactivity of diacyloxyiodobenzenes toward trivalent phosphorus nucleophiles
PublikacjaBadano reaktywność diacyloksyjodobenzenów w stosunku do nukleofilowych odczynników trójwiązalnego fosforu takich jak: fosforyny dialkilu, tlenki drugorzędowych fosfin oraz trzeciorzędowych fosfin.
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Reductive cleavage of the halogen-phosphorus and sulfur-phosphorus bonds with alkali metals
PublikacjaBadano redukcję chlorków kwasów tiofosforowych za pomocą: sodu lub potasu w ciekłym amoniaku i za pomocą antracenidku oraz naftalenidku potasu. Związki te ulegają, co wykazano, szybkiej redukcji do anionów >P-S- a te mogą być efektywnie utleniane siarką elementarną w ciekłym amoniaku.
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Isolation of collagen from the skins of Baltic cod (Gadus morhua).
PublikacjaBezbarwny kolagen wydzielono ze skór dorsza z ok. 90% wydajnością stosując trzykrotną, 24 godzinną ekstrakcję materiału 0.5 M roztworem kwasu cytrynowego, przy stosunku surowiec : rozpuszczalnik = 1 : 4. Stosując 0.5% dodatek niejonowych detergentów do roztworów ekstrahujących białka niekolagenowe ze skór uzyskuje się bezwonne izolaty kolagenu.
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Hydrophobic derivatives of 2-amino-2-deoxy-D-glucitol-6-phosphate: a newtype of D-glucosamine-6-phosphate synthase inhibitors with antifungal action.
PublikacjaDokonano syntezy szeregu N-acylowych i estrowych pochodnych 2-amino-2-deok-sy-glucitolo-6-fosforanu (ADGP) i zbadano ich aktywność przeciwgrzybową oraz wobec enzymów zaangażowanych we wczesne etapy biosyntezy chityny w komórkach grzybów. Wszystkie badane pochodne okazały się słabszymi inhibitorami enzymu syntezy GlcN-6-P aniżeli ADGP, ale niektóre z nich wykazywały znacznie wyższą aktywność przeciwgrzybową niż związek macierzysty....
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Chemically modified glass fiber as a matrix-free reference material for volatile compounds
PublikacjaW pracy opisano sposób wytwarzania nowego typu bezmatrycowych materiałów odniesienia lotnych związków organicznych. Do otrzymywania lotnych analitów wykorzystano technikę termicznego rozkładu związków powierzchniowych. Jako nośnik zastosowano modyfikowane chemicznie włókna szklane. Związkiem oznaczanym był chlorek metylu.
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Production of trehalose by intramolecular transglucosylation of maltose catalysed by a new enzyme from Thermus thermophilus hb-8
PublikacjaThermus thermophilus HB-8 jest źródłem syntazy trehalozy katalizującej konwersję maltozy. Aktywność specyficzna wytwarzania trehalozy w reakcji katalizowanej ekstraktem białek komórkowych wymienionej bakterii wynosi 0,1 U/mg białka i frakcjonowanie białek przez wysalanie siarczanem amonu powoduje około 3,5-krotne zwiększenie aktywności specyficznej. Optymalna temperatura konwersji maltozy wynosi 65 st.C i w 85 st.C zostaje zachowane...
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Synthesis, characterization and application of cross-linked functional terpolymer through epoxy group as sorbent for extraction of cadmium from waters and foods: Multivariate optimization
PublikacjaThe purpose of this study was to develop a selective sorbent for cadmium ions (Cd(II)) enrichment in orbital shaker assisted solid phase microextraction (OS-SPME) from different aqueous and food samples. A maleic anhydride-styrene-glycidyl methacrylate (MA-St-GMA) terpolymer was synthesized and characterized in detail. Experimental variables of sample preparation step were optimized using a central composite design (CCD). The final...
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Microplastics removal from aqueous environment by metal organic frameworks
PublikacjaThis paper provides an overview of recent research performed on the applications of metal–organic frameworks (MOFs) for microplastics (MPs) removal from aqueous environments. MPs pollution has become a major environmental concern due to its negative impacts on aquatic ecosystems and human health. Therefore, developing effective and sustainable methods for removing them from aqueous environments is crucial. In recent years, MOFs...
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How to make membrane distillation greener? A review on environmentally friendly and sustainable aspects
PublikacjaThere is an urgent need for the development of new water resources in order to solve the problem of the world’s growing demand for clean water. Membrane distillation (MD) is a promising alternative to conventional seawater desalination. Although MD itself is often defined as sustainable desalination technology, there are many aspects within the membrane manufacture and process operation that make it far from being green. For instance,...
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Isolation of Citrus lemon extracellular vesicles: Development and process control using capillary electrophoresis
PublikacjaA new and scalable method for the isolation of extracellular vesicles (EV) from Citrus lemon juice samples was developed. The methodology included preliminary preconcentration of the sample using ultrafiltration (UF) followed by size-exclusion chromatography (SEC) purification and final preconcentration of the eluates. Transmission electron microscopy and proteomic analysis showed that isolates contained exosome-like vesicles, exocyst-positive...
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Development of a vortex-assisted switchable-hydrophilicity solvent-based liquid phase microextraction for fast and reliable extraction of Zn (II), Fe (II), Pb (II), and Cd (II) from various baby food products
PublikacjaThis manuscript describes the development of a novel liquid phase microextraction (LPME) method for the extraction and determination of Zn (II), Fe (II), Pb (II), and Cd (II) in various infant/baby food and supplements products. The method is based on vortex-assisted extraction combined with a switchable-hydrophilicity solvent (SHS) sample preparation. The SHS, which undergoes reversible phase changes triggered by pH change, enables...
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Simple smartphone-based methods for the determination of bioactive compounds in wine
PublikacjaA set of simple smartphone-based methods of bioactive compounds determination were developed for wine analysis. Procedures for smartphone-based determination of the total content of phenolic compounds, flavonoids, anthocyanins and biogenic amines, as well as measurement of antioxidant activity were developed and fully validated. The experimental setup is based on smartphone and 3D-printed device, though it is very simple and can...
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Superconductivity–Electron Count Relationship in Heusler Phases─the Case of LiPd2Si
PublikacjaWe report superconductivity in the full Heusler compound LiPd2Si (space group Fm3̅m, No. 225) at a critical temperature of Tc = 1.3 K and a normalized heat capacity jump at Tc, ΔC/γTc = 1.1. The low-temperature isothermal magnetization curves imply type-I superconductivity, as previously observed in LiPd2Ge. We show, based on density functional theory calculations and using the molecular orbital theory approach, that while LiPd2Si...
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Investigation of use of hydrophilic/hydrophobic NADESs for selective extraction of As(III) and Sb(III) ions in vegetable samples: Air assisted liquid phase microextraction and chemometric optimization
PublikacjaIn this paper, a green, cost-effective sample preparation method based on air assisted liquid phase microextraction (AA-LPME) was developed for the simultaneous extraction of As(III) and Sb(III) ions from vegetable samples using hydrophilic/hydrophobic natural deep eutectic solvents (NADESs). Central composite design was used for the optimization of extraction factors including NADES volume, extraction cycle, pH, and curcumin concentration....
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Green, simple analytical method for total biogenic amines content determination in wine using spectrophotometry
PublikacjaA simple, green and equitable procedure for total biogenic amines (BAs) content determination was developed. The scientific novelty lies in the use of commercially available S 0378 dye, the reaction of which with BAs results in a colour change of the solution. Sample preparation and analysis were simplified to make the method suitable for routine analyses even in resource-scarce settings. The optimization of the method was carried...
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Probing Local Structural Changes by Sharp Luminescent Infrared Nanophosphor for Application in Light-Emitting Diodes
PublikacjaCr3+-doped infrared phosphors are promising candidates for next-generation phosphor-converted infrared light-emitting diodes (LEDs) because they can, in principle, tune and convert the luminescence spectra from an LED chip. However, most studies focus on broad-band Cr3+-doped phosphors, and the control mechanism of Cr3+-doped phosphors with sharp line emissions remains ambiguous. Here, we report LiGa5(1–x)Al5xO8:Cr3+ phosphors...
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Eu2Mg3Bi4: Competing Magnetic Orders on a Buckled Honeycomb Lattice
PublikacjaThe honeycomb lattice and its derived variants provide information on modeling and designing quantum magnets. A novel magnetic material, Eu2Mg3Bi4, which stabilizes in a previously unknown buckled honeycomb lattice, was discovered by high-pressure and high-temperature methods. We report here on the synthesis exploration of pure single crystals, structural determination of the buckled honeycomb lattice of europium moments, and experimental observation...
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Antiferromagnetic Order in the Rare-Earth Halide Perovskites CsEuBr3 and CsEuCl3
PublikacjaBulk CsEuBr3 and CsEuCl3 are experimentally shown to be magnetic semiconductors that order antiferromagnetically at Néel temperatures of 2.0 K and 1.0 K, respectively. Given that nanoparticles and thin films of CsEuCl3 have been reported to order ferromagnetically at a similar temperature, our observation of antiferromagnetic ordering in CsEuBr3 and CsEuCl3 expands the possible applications of halide perovskites to now include...
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Chemical Pressure Tuning Magnetism from Pyrochlore to Triangular Lattices
PublikacjaGeometrically frustrated lattices combined with magnetism usually host quantum fluctuations that suppress magnetic orders and generate highly entangled ground states. Three-dimensionally (3D) frustrated magnets generally exist in the diamond and pyrochlore lattices, while two-dimensionally (2D) frustrated geometries contain Kagomé, triangular, and honeycomb lattices. In this work, we reported using chemical pressure to tune the magnetism...
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Fe3–xInSnxO6 (x = 0, 0.25, or 0.5): A Family of Corundum Derivatives with Sn-Induced Polarization and Above Room Temperature Antiferromagnetic Ordering
PublikacjaThree new double corundum derivative compounds, Fe3−xInSnxO6 (x = 0. 0.25, or 0.5), were synthesized at high pressure and temperature (6 GPa and 1400− 1450 °C). All of the compounds order antiferromagnetically well above room temperature (TN = 608, 532, and 432 K for x = 0, 0.25, and 0.5, respectively). The x = 0 phase crystallizes as centrosymmetric R3̅c, but the inclusion of closed-shell d10 Sn4+ induces x = 0.25 and 0.5 to crystallize...
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A comprehensive review on Ginger (Zingiber officinale) as a potential source of nutraceuticals for food formulations: Towards the polishing of gingerol and other present biomolecules
PublikacjaCurrently, ginger is one the most consumed plants when dealing with the treatments of various illnesses. So far, it is known that various biologically active molecules, such as gingerols, shogaols and zingerone, among others, are the main responsible for specific biological activities, opening a new window for its utilization as a nutraceutical in foods. In pioneering extraction processes, solvent extraction has been initially...
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Phosphinophosphoranes: Mixed-Valent Phosphorus Compounds with Ambiphilic Properties
PublikacjaHerein, we present a simple synthesis of mixed-valent phosphinophosphoranes bearing three- and five-coordinate phosphorus centers. Compounds with phosphorus–phosphorus bonds were synthesized via a reaction of lithium phosphides RR′PLi with cat2PCl (cat = catecholate), whereas derivatives with methylene-linked phosphorus centers were obtained via a reaction of phosphanylmethanides RR′CH2Li with cat2PCl. The presence of accessible...
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Organic solvents aggregating and shaping structural folding of protein, a case study of the protease enzyme
PublikacjaLow solubility of reactants or products in aqueous solutions can result in the enzymatic catalytic reactions that can occur in non-aqueous solutions. In current study we investigated aqueous solutions containing different organic solvents / deep eutectic solvents (DESs) that can influence the protease enzyme's activity, structural, and thermal stabilities. Retroviral aspartic protease enzyme is responsible for the cleavage of the...
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Online Volatile Compound Emissions Analysis Using a Microchamber/Thermal Extractor Coupled to Proton Transfer Reaction-Mass Spectrometry
PublikacjaIndoor air is a complex and dynamic mixture comprising manifold volatile organic compounds (VOCs) that may cause physiological and/or psychological discomfort, depending on the nature of exposure. This technical note presents a novel approach to analyze VOC emissions by coupling a microchamber/thermal extractor (μ-CTE) system to a proton transfer reaction-mass spectrometer (PTR-MS). This configuration provides an alternative to...
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Group-9 Transition-Metal Suboxides Adopting the Filled-Ti2Ni Structure: A Class of Superconductors Exhibiting Exceptionally High Upper Critical Fields
PublikacjaTi2Ni and the related η-carbide structure are known to exhibit various intriguing physical properties. The Ti2Ni structure with the cubic space group Fd3̅m is surprisingly complex, consisting of a unit cell with 96 metal atoms. The related η-carbide compounds correspond to a filled version of the Ti2Ni structure. Here, we report on the structure and superconductivity in the η-carbide-type suboxides Ti4M2O with M = Co, Rh, and Ir....
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Amberlyst-15 catalysed synthesis of novel indole derivatives under ultrasound irradiation: Their evaluation as serotonin 5‑HT2C receptor agonists
PublikacjaA series of indole based novel Schiff bases was designed as potential agonists of 5‑HT2C receptor that was supported by docking studies in silico. These compounds were synthesized via Amberlyst-15 catalysed condensation of an appropriate pyrazole based primary amine with the corresponding indole-3-aldehyde under ultrasound irradiation at ambient temperature. A number of target Schiff bases were obtained...
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The content of biogenic amines in Rondo and Zweigelt wines and correlations between selected wine parameters
PublikacjaThe purpose of this study was to evaluate the content of biogenic amines (BAs) in wines using dispersive liquid–liquid microextraction–gas chromatography–mass spectrometry (DLLME-GC–MS). An additional objective was to assess the correlations between selected parameters characterizing the samples such as the content of BAs, sugars, and organic acids, pH, and total acidity. Wines produced from the same grape variety in which alcoholic...
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Complementary green analytical procedure index (ComplexGAPI) and software
PublikacjaIt is not easy to find appropriate tools for the evaluation of the “green”nature of analytical methodologies which involve the use of compounds, materials, or chemicals manufactured prior to the analytical step. Here, we propose a new metric for the evaluation of analytical procedures based on the GAC attributes. The proposed solution expands on the well-known green analytical procedure index by adding additional fields pertaining...
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Effect of convection and microwave heating on the retention of bioactive components in human milk
PublikacjaBioactive substances are very important components of human milk (HM), especially for premature newborns. The effects of convection (CH) and microwave heating (MWH) at 62.5 and 66 °C, on the level of selected bioactive components of HM: lysozyme (LZ), lactoferrin (LF), secretory immunoglobulin A (sIgA), basal lipase (BL), cytokine TGF-2, vitamin C and total antioxidant capacity (TAC) was compared. Regardless of the used heating methods...
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Chromium‑based metal organic framework for pipette tip micro‑solid phase extraction: an effective approach for determination of methyl and propyl parabens in wastewater and shampoo samples
PublikacjaAbstract Background A chromium-based metal organic framework was synthesized and employed as an efficient sorbent for pipette tip micro-solid phase extraction and preconcentration of parabens from wastewater and shampoo samples up to sub-ppb level before their spectrophotometric analysis. Results Factors affecting preconcentration including volume and type of solvent, amount of sorbent, number of extraction, and volume and pH of...
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A method for a comprehensive lipidomic analysis of flaxseed (Linum usitatissimum) with the use of LC–Q-TOF-MS and dispersive micro-solid-phase (μDSPE) extraction
PublikacjaFlaxseed (FS) is one of the richest sources of α-linolenic acid oil and lignans, and it is suggested that the consumption of flaxseed may contribute to the prevention of certain chronic diseases such as many types of cancer, diabetes, cardiovascular diseases and cerebrovascular stroke. Here, we demonstrate a new method for comprehensive FS lipidome profiling with the use of LC–Q-TOF-MS and dispersive micro-solid-phase extraction....