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Wyniki wyszukiwania dla: CHIRAL DERIVATIZATION
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Circular Dichroism Imaging: Mapping the Local Supramolecular Order in Thin Films of Chiral Functional Polymers
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New chiral discotics with helical organization of the mesophase—liquid crystalline derivatives of dibenzotetraaza[14]annulene
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Application of the 2-deoxyglucose scaffold as a new chiral probe for elucidation of the absolute configuration of secondary alcohols
PublikacjaHerein, we present the application of 2-deoxy-D-glucose derivatives as chiral probes for elucidation of the absolute configuration of chiral secondary alcohols. The probes are attached to the studied molecules via glycosylation reaction and the resulting products are examined by a set of standard 2D NMR experiments. The absolute configuration of an oxymethine carbon atom binding the probe is established on a basis of a set of diagnostic...
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Planar chiral dianthranilide and dithiodianthranilide molecules: optical resolution, chiroptical spectra, and molecular self-assembly.
PublikacjaChiralny planarnie diantranilid został rozdzielony na enancjomery przy użyciu chlorku (-)-(1S,4R)-kamfanoilu. Konfigurację absolutną (S)-enancjomeru ustalono na podstawie analizy rentgenograficznej monokryształu jego N,N'-dikamfoilopochodnej. Natomiast rozdział ditiodiantranilidu na enancjomery przeprowadzono poprzez tworzenie związków inkluzyjnych z (R,R)-1,2-diaminocykloheksanem. Otrzymanemu w ten sposób enancjomerowi przypisano...
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Common methods for the chiral determination of amphetamine and related compounds I. Gas, liquid and thin-layer chromatography
PublikacjaThis article reviews the most common, useful methods for the chiral determination of amphetamine (AM) and AM-deriveddesigner drugs in different of matrix, including blood, hair, urine, medicaments or standard solutions, taking into considerationarticles published in the past 15 years. We consider chromatographic methods (e.g., gas, liquid, high-performance liquid, and thinlayer). We describe several types of chiral derivatization...
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The optimisation of analytical parameters for routine profiling of antioxidants in complex mixture by HPLC coupled post-column derivatisation
PublikacjaIntroduction: The wide application of natural and artificial antioxidants in food, cosmetic and pharmaceutical industry as well as the recognition of the importance of food antioxidants for supporting human health created demand for reliable and industrially applicable methods of determining antioxidative activity. This requirement can be fullfilled with the recently proposed HPLC-post-column derivatisation approach enabling the...
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Common methods for the chiral determination of amphetamine and related compounds II: Capillary electrophoresis and nuclear magnetic resonance
PublikacjaAmphetamine group and related ring-substituted substances are generally synthetic compounds, belonging to one of the most heavily abused drug groups in recent years. Some compounds in this class also originate from plants. Analysis of the enantiomers of AM-type compounds and metabolites is extremely important for a number of scientific disciplines. From studies of biological activity or mechanisms through determination of precursor...
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Electronic circular dichroism imaging (CDi) maps local aggregation modes in thin films of chiral oligothiophenes
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TaRh 2 B 2 and NbRh 2 B 2 : Superconductors with a chiral noncentrosymmetric crystal structure
PublikacjaIt is a fundamental truth in solid compounds that the physical properties follow the symmetry of the crystal structure. Nowhere is the effect of symmetry more pronounced than in the electronic and magnetic properties of materials—even the projection of the bulk crystal symmetry onto different crystal faces is known to have a substantial impact on the surface electronic states. The effect of bulk crystal symmetry on the properties...
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Determination of β-blockers and β-agonists using gas chromatography and gas chromatography–mass spectrometry – A comparative study of the derivatization step
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Capillary gas chromatography using a -cyclodextrin forenantiomeric separation of methylamphetamine, its precursors andchloro intermediates after optimization of the derivatization reaction
PublikacjatThe enantiomeric ratio of methylamphetamine (MAMP) is closely related to the optical activity of precur-sors and reagents used for the synthesis and this knowledge can provide useful information concerningthe origins and synthetic methods used for illicit manufacture. The information can be utilized for reg-ulation of the precursors and investigation of the manufacturing sources but this requires analyticalprocedures to determine...
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Simultaneous determination of individual isothiocyanates in plant samples by HPLC-DAD-MS following SPE and derivatization with N-acetyl-l-cysteine
PublikacjaThe procedure for the isothiocyanates (ITCs) determination that involves derivatization with N-acetyl-l-cysteine (NAC) and separation by HPLC was developed. Prior to derivatization, plant ITCs were isolated and purified using solid-phase extraction (SPE). The optimum conditions of derivatization are: 500 μL of isopropanolic eluate obtained by SPE combined with 500 μL of derivatizing reagent (0.2 M NAC and 0.2 M NaHCO3 in water)...
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HS-SPME-CGC-PID determination of aldehydes in rectified spirits and vodkas after derivatisation with 2,4,6-trichlorophenylhydrazine (TCPH)
PublikacjaW pracy przedstawiono nową metodę oznaczania aldehydów w spirytusach i wyrobach spirytusowych czystych z zastosowaniem 2,4,6-trichlorofenylohydrazyny (TCPH) jako odczynnika derywatyzującego. Zaproponowana metoda jest co najmniej 100-krotnie tańsza od mikroekstrakcji do fazy stacjonarnej z fazy nadpowierzchniowej (HS-SPME) i chromatografii gazowej z zastosowaniem często zalecanej o-2,3,4,5,6-pentafluorobenzylohydroxyloaminy (PFBHA)....
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An integrated geotechnical and geophysical investigation of landslide in Chira town, Ethiopia
PublikacjaLandslides pose a significant threat to infrastructure, property, and human lives in many regions worldwide, including Chira town in Ethiopia. This study presents an integrated geotechnical and geophysical investigation aimed at identifying the contributing factors to landslides in Chira town, Ethiopia, with a focus on a recent landslide event. The methodology employed a combination of geotechnical and geophysical techniques to...
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Syntheses, structures, and chiroptical and magnetic properties of chiral clusters built from Schiff bases: a novel [MnIIMnIII6NaI2] core
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Chiral Pyrazolo[4,3-e][1,2,4]triazine Sulfonamides—Their Biological Activity, Lipophilicity, Protein Affinity, and Metabolic Transformations
PublikacjaReferring to our previous laboratory results related to the tyrosinase and urease inhibition by pyrazolo[4,3-e][1,2,4]triazine sulfonamides, we examined here in silico the mechanism of action at the molecular level of the investigated pyrazolotriazine sulfonamides by the molecular docking method. The studied compounds being evaluated for their cytotoxic effect against cancer cell lines (MCF-7, K-562) and for recombinant Abl and...
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A rapid spectrofluorimetric method for the determination of malondialdehyde in human plasma after its derivatization with thiobarbituric acid and vortex assisted liquid–liquid microextraction
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Determination of amikacin and ciprofloxacin by liquid chromatography with pre-column derivatization to evaluate sustained delivery of antibiotics from Drug-Eluting Biopsy Needle
PublikacjaDetermination of chosen antibacterial antibiotics: amikacin and ciprofloxacin was carried out by HPLC-UV after derivatization with 9-fluorenylmethyl chloroformate and in their native form by HPLC-MS/MS. Developed methods have been applied to control the kinetics of antibiotic release from polymer-based controlled drug delivery system.
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Novel fast analytical method for indirect determination of MCPD fatty acid esters in edible oils and fats based on simultaneous extraction and derivatization
PublikacjaA novel method for indirect determination of MCPD esters levels in lipid samples has been developed. The method is based on combination of extraction and derivatisation in the same sample preparation step. It is achieved by the application of diethyl ether as extraction solvent for isolation of released from esterified forms analytes from water phase and dilution solvent for solid PBA – derivatisation agent. It is a noteworthy...
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Enantioselective Extraction System Containing Binary Chiral Selectors and Chromatographic Enantioseparation Method for Determination of the Absolute Configuration of Enantiomers of Cyclopentolate
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Method for the determination of carboxylic acids in industrial effluents using dispersive liquid-liquid microextraction with injection port derivatization gas chromatography–mass spectrometry
PublikacjaThe paper presents a new method for the determination of 15 carboxylic acids in samples of postoxidative effluents from the production of petroleum bitumens using ion-pair dispersive liquid-liquid microextraction and gas chromatography coupled to mass spectrometry with injection port derivatization. Several parameters related to the extraction and derivatization efficiency were optimized. Under optimized experimental conditions,the...
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Application of safirinium N-hydroxysuccinimide esters to derivatization of peptides for high-resolution mass spectrometry, tandem mass spectrometry, and fluorescent labeling of bacterial cells
PublikacjaMass spectrometry methods are commonly used in the identification of peptides and biomarkers. Due to a relatively low abundance of proteins in biological samples, there is a need for the development of novel derivatization methods that would improve MS detection limits. Hence, novel fluorescent N-hydroxysuccinimide esters of dihydro-[1,2,4]triazolo[4,3-a]pyridin-2-ium carboxylates (Safirinium P dyes) have been synthesized. The...
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Helicity discrimination in N,N'-dibenzoyl-1,2,3,4,7,8,9,10-octahydro-1,10-phenanthrolines and their thiono- and selenocarbonyl analogues by inclusion complexation with chiral diols
PublikacjaX-ray crystallographic analysis of the title compounds revealed that they assume a folded helical con- formation of an approximate C2 symmetry in the solid state. Dithioamide, diselenoamide and monoselenoamide were resolved to enantiomers by inclusion crystallization with optically active diols (TADDOLs). The absolute configuration of the guest molecules in the complexes was assigned as P. The optical activity of the resolved compounds...
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Molecular geometry and optical activity of helically chiral N-nitrosamines derived from 1,2,3,4-tetrahydro- and 1,2,3,4,7,8,9,10-octahydro-1,10-phenanthroline
PublikacjaX-ray crystallographic analysis of the title N-nitrosamines revealed that they assume helical conformations in the solid state. Nitrosamines 1b and 2b were resolved by inclusion crystallization with optically active diols (TADDOLs). The absolute configuration of the guest molecules in the complexes 1b·3b and 2b·3b was assigned as M. The optical activity of the resolved compounds is manifested by their solid state CD spectra, which...
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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
PublikacjaIn 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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Copper(I) halide cluster-based coordination polymers modulated by chiral ditopic dithiodianthranilide ligands: synthesis, crystal structure and photoluminescence
PublikacjaReaction of copper(I) halides with chiral dithiodianthranilidesmdtaandbdtaafforded polymeric complexeswhere polynuclear CuX clusters were linked together by ditopic bridging ligands into 1D chains or 2D layerstructures. In the case of racemic ligands double stranded chain polymers were formed where the Cu4X4(X = I or Br) cores are connected by enantiomeric pairs of the ditopic ligands. In contrast, a homochiralmdtaligand created...
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Determination of pharmaceutical residues in drinking water in Poland using a new SPE-GC-MS(SIM) method based on Speedisk extraction disks and DIMETRIS derivatization
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An in situ derivatization – dispersive liquid–liquid microextraction combined with gas-chromatography – mass spectrometry for determining biogenic amines in home-made fermented alcoholic drinks
PublikacjaA novel dispersive liquid–liquid microextraction (DLLME) gas chromatography mass-spectrometry(GC–MS) method was developed for the determination of 13 biogenic amines in home-made wine sam-ples. The method allows to simultaneous extraction and derivatization of the amines providing a simpleand fast mode of extract enrichment. During the study, two different procedures were examined. Sta-tistical analysis was performed to choose...
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A novel method of local chirp-rate estimation of LFM chirp signals in the time-frequency domain
PublikacjaIn the paper, novel dynamic representations of a complex signal in the time-frequency domain are introduced. The proposed approach is based on using the gradient of the short-time Fourier transform complex phase. A channelized instantaneous complex frequency (CICF) and a complex local group delay (CLGD) are included in the presented signal representations. An application of the newly-introduced distributions is demonstrated by...
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Phenolic composition and antioxidant properties of polish blue-berried honeysuckle genotypes by HPLC-DAD-MS, HPLC postcolumn derivatization with ABTS or FC, and TLC with DPPH visualization
PublikacjaIn this study, different Polish cultivars of blue-berried honeysuckles (Lonicera caerulea L.), wild and bog bilberry, were analyzed for bioactive compounds. The chemical properties verified included composition of anthocyanins and other polyphenols, antioxidant activity, and profiles of antioxidants by HPLC postcolumn derivatization or TLC. The antioxidant activities of different blue-berried honeysuckle cultivars were similar...
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Sample preparation procedure using extraction and derivatization of carboxylic acids from aqueous samples by means of deep eutectic solvents for gas chromatographic-mass spectrometric analysis
PublikacjaThe paper presents a new procedure for the determination of organic acids in a complex aqueous matrixusing ultrasound-assisted dispersive liquid–liquid microextraction followed by injection port derivati-zation and GC–MS analysis. A deep eutectic solvent (choline chloride: 4-methylphenol in a 1:2 mol ratio)was used both as an extracting solvent and as a derivatizing agent to yield ion pairs which were next con-verted to methyl...
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Effects of Surface Energy and Surface Residual Stresses on Vibro-Thermal Analysis of Chiral, Zigzag, and Armchair Types of SWCNTs Using Refined Beam Theory
PublikacjaIn this article, vibration characteristics of three different types of Single-Walled Carbon Nanotubes (SWCNTs) such as armchair, chiral, and zigzag carbon nanotubes have been investigated considering the effects of surface energy and surface residual stresses. The nanotubes are embedded in the elastic substrate of the Winkler type and are also exposed to low and high-temperature environments. A new refined beam theory namely, one-variable...
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A new silylating reagent – dimethyl(3,3,3-trifluoropropyl)silyldiethylamine – for the derivatisation of non-steroidal anti-inflammatory drugs prior to gas chromatography–mass spectrometry analysis
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A novel methodology for the enantiomeric resolution of methamphetamine, its precursors and intermediates by 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 from this 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. In this study, simultaneous chiral separation of methylamphetamine,...
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Front Cover: Chiral Molecular Cages Based on Cyclotriveratrylene and Sucrose Units Connected with p ‐Phenylene Linkers (Eur. J. Org. Chem. 6/2021)
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The Scuffing Resistance of WC/C Coated Spiral Bevel Gears
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Intra-provincial inequalities and economic growth in China
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China and the Chinese in the modern world. An interdisciplinary study
PublikacjaThis monograph is a collection of chapters devoted to modern China on various approaches. There is no future without a past and a modern China is a country that skillfully combines the new with the old and the authors have attempted to present this phenomenon in this book. It brings to light issues such as a honorificativity in Chinese administrative and legal documents, a comparison of Chinese and...
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Viral Infections and Cancer During Alcohol Use
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Determination of heavy metals in eyeshadows from China
PublikacjaPersonal care products and cosmetics are used daily by many people, causing local exposure to certain chemical substances through the application directly inside the oral cavity, on the skin, lips, eyes, and mucosa. Eyeshadows are among the most commonly used types of cosmetics. According to scientifc reports, they may contain heavy metals, especially in non-original products. The exposure to said heavy metals may cause local skin...
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FOREIGN TRADE WITH CHINA: NO REASON FOR “GERMAN ANGST”
PublikacjaSankcje w związku z rosyjską agresją zbrojną przeciwko Ukrainie i naruszenie zwykłych światowych szlaków handlowych powodują w Niemczech obawy, że niemiecka gospodarka może zostać szantażowana handlem z silnym partnerem, tj. Chinami.Analiza danych dotyczących niemiecko-chińskiego handlu zagranicznego i jego wpływu na gospodarkę i zatrudnienie pokazuje, że Chiny są jednym z nielicznych...
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Chiralne katalizatory tiomocznikowe w reakcji stereoselektywnego alkilowania związków heteroaromatycznych
PublikacjaNiniejsza praca doktorska podzielona jest na trzy zasadnicze części: wstęp teoretyczny, badania własne oraz część eksperymentalną. Studium literaturowe obejmuje przegląd doniesień z ostatnich lat z dziedziny organokatalizy niekowalenycjnej. Zaprezentowano zakres zastosowań organokatalizatorów tiomocznikowych jednofunkcyjnych i dwufunkcyjnych z uwzględnieniem ograniczeń w strukturze reagentów, roli dodatków katalitycznych i mechanizmu...
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Elemental characteristics of mushroom species cultivated in China and Poland
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Determination of electrode impedance by means of exponential chirp signal
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Determination of electrode impedance by means of exponential chirp signal.
PublikacjaPrzedstawiona została nowa metoda pomiaru impedancji elektrodowej. Jako pobudzenie zastosowany został niestacjonarny sygnał napięciowy, którego częstotliwość jest ekspotencjalną funkcją czasu. Zastosowanie zmodyfikowanej któtko-czasowej transformaty Fouriera (STFT) w analizie napięciowego pobudzenia i odpowiedzi prądowej pozwala na otrzymanie widma impedancyjnego.
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Efficacy of intralesional bleomycin in treatment resistant viral warts
PublikacjaIntroduction Optimal management of treatment-refractory viral warts caused by human papillomavirus is unknown. One of the treatment methods is intralesional bleomycin solution. Objective To determine risk factors for resistant viral warts (not responding to conventional treatments for ≥ 6 months), to determine the effectiveness and safety of intralesional bleomycin in a group of patients with viral warts resistant to conventional...
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Economic significance of initial public offerings in China and India
PublikacjaRapid economic growth in China and India has attracted attention of many researchers, focusing on various social and economic factors underlying the success of these countries. One of the key components of country’s economy is financial system which consists of segments such as banking sector and equity market. The topic of initial public offerings (IPOs), one of the corporate financing sources, involving raising funds through...
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Monosaccharides as internal probes for the determination of the absolute configuration of 2-butanol
PublikacjaD-dlukoza, D-mannoza i L-ramnoza zostały poddane reakcji z mieszaniną racemiczną 2-butanolu. Otrzymane w ten sposób glikozydy były analizowane za pomocą spektroskopii NMR, z wykorzystaniem eksperymentów COSY i NOESY. Analiza konformacyjna wiązania glikozydowego (dokonana w oparciu o modelowanie molekularne i heteronuklearne stałe sprzężenia) wraz z analizą sprzężeń dipolowych obserwowanych w widmie NOESY umożliwiła określenie konfiguracji...
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New thiourea organocatalysts and their application for the synthesis of 5-(1H-indol-3-yl)methyl-2,2-dimethyl-1,3-dioxane-4,6-diones a source of chiral 3-indoylmethyl ketenes
PublikacjaThe stereoselective properties of modified thiourea organocatalysts were tested in the Friedel–Crafts alkylation of indole with 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones, which produces chiral 5-((1H-indol-3-yl)(aryl)methyl)-2,2-dimethyl-1,3-dioxane-4,6-diones. Based on a tentative reaction mechanism for ((S)-N-benzyl-2-(3-(3,5-bis (trifluoromethyl)phenyl)thioureido)-N,3,3-trimethylbutanamide organocatalysts, modifications...
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The Role of NF-κB in Uterine Spiral Arteries Remodeling, Insight into the Cornerstone of Preeclampsia
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