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81.
The use of high pressure for the enzymatic synthesis of pharmacologically interesting molecules is a very important tool. Hesperidin and hesperitin exhibit anti-inflammatory, antimicrobial, antioxidant, and anticarcinogenic properties and prevent bone loss. However, hesperidin has a low bioavailability compared with hesperitin, due to the rutinoside moiety attached to the flavonoid. The aim of this work was the enzymatic production of hesperitin from hesperidin (soluble and insoluble) with hesperidinase free and immobilized in Ca-alginate beads, under high pressure conditions. The work was focused on the optimization of enzyme activity, studying the effects: pressure (50–150 MPa), temperature (35–75 °C), concentration of substrate (100–800 mg/L), and immobilization of hesperidinase. An 18-fold increase in hesperidinase residual activity was observed under high pressure conditions of 100 MPa compared to 0.1 MPa. A higher specificity of the hydrolytic reaction under high pressure (100 MPa) with a two-and three-fold increase in the ratio K cat/K M (specificity constant) at 55 °C and 75 °C was observed. A two-fold increase in the maximum activity at 100 MPa was observed with immobilized hesperinase compared to 0.1 MPa. In the second reutilization, almost a four-fold increase was obtained under high pressure conditions in comparison to atmospheric pressure. 相似文献
82.
Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography and mass spectrometry (GC-MS) was applied to the determination of six organophosphorous pesticides (OPPs) in water samples. The analytes included in this study were prophos, diazinon, chlorpyrifos methyl, methyl parathion, fenchlorphos and chlorpyrifos. Several extraction and dispersion solvents were tested for dispersive liquid-liquid microextraction of these analytes and the best results were obtained using chloroform as extraction solvent and 2-propanol as dispersion solvent. Calibration curves of the analytes in water samples were constructed in the concentration range from 100 to 1100 ng/L for prophos, diazinon and methyl parathion and in the range from 100 to 1000 ng/L for chlorpyrifos methyl, fenchlorphos and chlorpyrifos. Limits of detection (LODs) were in the range of 1.5-9.1 ng/L and limits of quantification (LOQs) were in the range of 5.1-30.3 ng/L, below the maximum admissible level for drinking water. Relative standard deviations (RSDs) were between 6.5 and 10.1% in the concentration range of 100-1000 ng/L. The relative recoveries (%RRs) of tap, well and irrigation water samples fortified at 800 ng/L were in the range of 46.1-129.4%, with a larger matrix effect being detected in tap water. 相似文献
83.
Patel SM de la Fuente M Ke S Guimarães AM Oliyide AO Ji X Stapleton P Osbourn A Pan Y Bowles DJ Davis BG Schatzlein A Yang M 《Chemical communications (Cambridge, England)》2011,47(38):10569-10571
Glycosylated analogues of novobiocin, discovered using a broad library of enzymes, have 100-fold improved activity against breast, brain, pancreatic, lung and ovarian cancers and ablated associated off-target activity leading to an up to 2.7 × 10(4) fold increase in selectivity. 相似文献
84.
The synthesis of (E)-3-(meso-octamethylcalix[4]pyrrol-2-yl)propenal and its use in Knoevenagel reactions are described. The resulting compounds display sharp changes in color in the presence of fluoride, acetate, and dihydrogen phosphate anions. 相似文献
85.
Prof. Fernanda Andreia Rosa Samara Mendes de Souza Melo Dr. Karlos Eduardo Pianoski Julia Poletto Mariellen Guilherme dos Santos Dr. Michael Jackson Vieira da Silva Dr. Danielle Lazarin-Bidóia Dr. Hélito Volpato Prof. Sidnei Moura Prof. Celso Vataru Nakamura 《ChemistryOpen》2021,10(10):931-938
A series of 60 4-aminomethyl 5-aryl-3-substituted isoxazoles were synthesized by an efficient method and evaluated in vitro against Leishmania amazonensis and Trypanosoma cruzi, protozoa that cause the neglected tropical diseases leishmaniasis and Chagas disease, respectively. Thirteen compounds exhibited a selective index greater than 10. The series of 3-N-acylhydrazone isoxazole derivatives bearing the bithiophene core exhibited the best antiparasitic effects. 相似文献
86.
Andreia LeiteAna M.G. Silva Ana NunesMariana Andrade Carla SousaLuís Cunha-Silva Paula GameiroBaltazar de Castro Maria Rangel 《Tetrahedron》2011,67(22):4009-4016
The synthesis and characterization of three novel tetradentate ligands (T1, T2 and T3) based on 3-hydroxy-4-pyridinone chelating units are described. The three ligands exhibit different flexibility due to the use of two different anchor molecules, piperazine and 1,2-diaminobenzene, and to the diverse length of the 3-hydroxy-4-pyridinone arms. All reactions were performed using both conventional heating and microwave irradiation in order to evaluate the possibility of using greener methods in these synthetic procedures. The results showed that, in all cases, microwave irradiation provides the desired ligands reducing reaction time in ca. 97%. The structure of ligand T3 was resolved by X-ray crystallography, showing significant hydrogen bonding and interesting π-π interaction between the benzene and pyridinone rings. The use of potentiometric and spectroscopic methods allowed determination of acidity constants and unequivocal assignment of proton loss for each pKa value. Interaction of the ligands with divalent metal ions was assessed by spectroscopic methods. 相似文献
87.
Attila TakácsAntal Szilágyi Péter ÁcsLászló Márk Andreia F. PeixotoMariette M. Pereira László Kollár 《Tetrahedron》2011,67(13):2402-2406
Various 5-carboxamido-7-iodo-8-benzyloxyquinolines were synthesised via selective aminocarbonylation of 5,7-diiodo-8-benzyloxyquinoline in the presence of ‘in situ’ generated palladium(0) catalysts. Under similar conditions (50 °C, 80 bar CO), 5,7-bis(N-tert-butyl-glyoxylamido)-8-hydroxyquinoline was obtained using tert-butylamine as N-nucleophile. The unprotected 5,7-diiodo-8-hydroxyquinoline underwent dehydroiodination resulting in 8-hydroxyquinoline as the major product. 相似文献
88.
Immobilized Laccase on a New Cryogel Carrier and Kinetics of Two Anthraquinone Derivatives Oxidation
Stanescu MD Sanislav A Ivanov RV Hirtopeanu A Lozinsky VI 《Applied biochemistry and biotechnology》2011,165(7-8):1789-1798
A coordinatively immobilized laccase was prepared using a new cryogel type carrier. The support has a wide-pore texture facilitating diffusion of different substrates to the enzyme reaction center. The biocatalyst proved to be efficient in decolorization of two anthraquinone derivatives, namely Acid Blue 62 and bromaminic acid. After 24 h over 80% of the two substrates have been oxidated. The kinetic data (K (m) and V (max)) for the oxidation of the two anthraquinone derivatives, with the free and immobilized enzyme, have been determined and compared. Other parameters, like k (cat) and the specificity constant have been calculated and analyzed. The influence of substrate properties (hydrophobicity, polarity, etc.) has been discussed. 相似文献
89.
Silva AM Borralho AC Pinho SA Domingues MR Domingues P 《Rapid communications in mass spectrometry : RCM》2011,25(10):1413-1421
Peptide and protein lipoxidation is a deleterious process which has been related to several degenerative conditions. In the present study, the interaction of lipid secondary oxidation products with peptides was investigated by evaluating the modifications occurring to angiotensin II (Ang-II) in the presence of an oxidizing polyunsaturated glycerophospholipid (1-palmitoyl-2-arachidonoyl-glycerophosphatidylcholine, PAPC). PAPC oxidation was promoted by Fenton chemistry and the oxidation products were incubated with Ang-II. The reaction products were finally analysed by off-line nanospray high-performance liquid chromatography/matrix-assisted laser desorption/ionization tandem mass spectrometry (nano-HPLC/MALDI-TOF-MS/MS). Ang-II was found to form adducts with 26 different aldehydes, leading to 37 distinct reaction products. Modification of Ang-II occurred through reaction with reactive carbonyl species (RCS) originating from fatty acyl chain cleavage, while interactions with the oxidized phospholipid could not be detected. Adduction was observed to occur both by Michael and Schiff base mechanisms, most prevalently taking place at the peptide N-terminus or the arginine residue. Histidine modification could only be demonstrated to occur via Michael addition with two aldehydes: 4-hydroxy-2-nonenal (HNE) and 2-octenal. The highly reactive 4-oxo-2-nonenal (ONE) was shown to react preferentially with the arginine side chain, while malondialdehyde addition could only be confirmed at the N-terminus. Aspartic acid oxidative decarboxylation, amino acid side chain oxidation, multiple adduction or peptide cross-links could not be perceived. The inability to detect these reaction products is indicative of their low abundance or non-existence in competitive reaction conditions. The multiplicity of peptide modifications described emphasizes the complexity of lipoxidation, the effects of which are not possible to fully understand by the evaluation of independent reaction products. 相似文献
90.
Alexandre Rodrigues M. Cidália R. Castro Andreia S.F. Farinha Manuel Oliveira João P.C. Tomé Ana V. Machado M. Manuela M. Raposo Loic Hilliou Gabriel Bernardo 《Polymer Testing》2013
The thermal stability of poly(3-hexylthiophene) (P3HT) in its molten state was investigated in air and nitrogen atmospheres under no illumination conditions, with the aim of testing the feasibility of processing it using polymer melt techniques. A large set of different experimental characterization techniques was used including thermogravimetric analysis (TGA), rotational rheometry, infrared spectroscopy (FTIR-ATR), proton nuclear magnetic resonance spectroscopy (1H-NMR), gel permeation chromatography (GPC), UV-Vis and fluorescence spectroscopy. The results obtained strongly suggest that the processing of P3HT in its molten state is possible, without noticeable degradation, if carried out under nitrogen atmosphere and if the processing (residence) times are relatively short. Conversely, as expected, in a normal air atmosphere P3HT degrades rapidly at temperatures above its melting point. The effect of PCBM on the thermal stability of P3HT:PCBM blends in the molten state was also studied using TGA, and in air atmosphere PCBM is shown to delay oxidation. 相似文献