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1.
F. Zehra Küçükbay Nesrin Buğday Claudiu T. Supuran 《Journal of enzyme inhibition and medicinal chemistry》2016,31(6):1221-1225
N-protected amino acids were reacted with substituted benzothiazoles to give the corresponding N-protected amino acid-benzothiazole conjugates (60–89%). Their structures were confirmed by proton nuclear magnetic resonance (1H NMR), carbon-13 nuclear magnetic resonance (13C NMR), IR and elemental analysis. Their carbonic anhydrase (CA, EC 4.2.1.1) inhibitory activities were determined against two cytosolic human isoforms (hCA I and hCA II), one membrane-associated (hCA IV) and one transmembrane (hCA XII) enzyme by a stopped-flow CO2 hydrase assay method. The new compounds showed rather weak, micromolar inhibitory activity against most of these enzymes. 相似文献
2.
Sequential resonance assignments in protein 1H nuclear magnetic resonance spectra. Basic pancreatic trypsin inhibitor 总被引:24,自引:0,他引:24
The assignment of the 1H nuclear magnetic resonance spectrum of the basic pancreatic trypsin inhibitor with the use of two-dimensional 1H nuclear magnetic resonance techniques at 500 MHz is described. The assignments are based entirely on the known amino acid sequence and the nuclear magnetic resonance data. Individual resonance assignments were obtained for all backbone and Cβ protons, with the exception of those of Arg1, Pro2, Pro13 and the amide proton of Gly37. The side-chain resonance assignments are complete, with the exception of Pro2 and Pro13, the Nδ protons of Asn44 and the peripheral protons of the lysine residues and all but two of the arginine residues. 相似文献
3.
G. Victor Fazakerley Andre Guy Robert Teoule Wilhelm Guschlbauer 《Journal of biosciences》1985,8(3-4):537-552
We have studied the conformation of two hexanucleotides d(GGATCC) and d(GGm6ATCC) using proton nuclear magnetic resonance. Nuclear Overhauser effect measurements show that d(GGATCC) assumes a normal
right handed B helix. The single and double strand resonances are in fast exchange on a proton nuclear magnetic resonance
time scale. For d(GGm6ATCC), up to the Tm separate resonances are observed for each state, indicating slow exchange, though above the Tm it becomes
more rapid. The orientation of the adenosine methyl-amino group, preferentiallycis to N1, hinders base pair formation.The connectivities of the resonances of the two states were established by saturation transfer
experiments. At 0°C irradiation of the m6 A-T imino proton gives an nuclear Overhauser effect to AH2 showing that base pairing is Watson-Crick. Intra and interresidue nuclear Overhauser effects starting from the 3′ terminus
show that the helix is right handed and in the B-form.The results on the two oligomers demonstrate that adenosine methylation
induces little or no change in the conformation of the helix, but reduces the Tm from 45° to 32°C and slows the opening and
closing of the m6A.T base pair by a factor of about 100. 相似文献
4.
Gérard Strecker Jean-Michel Wieruszeski Claude Martel Jean Montreuil 《Glycoconjugate journal》1987,4(4):329-337
Alkaline borohydride reductive cleavage of hen ovomucin resulted in the release of a series of neutral and acidic oligosaccharide-alditols.1H-NMR spectroscopy in combination with fast ion bombardment-mass spectrometry in negative ion mode were used for investigation of the structures of three oligosaccharide-alditols. The following structures were established:
Abbreviations NeuAc
N-acetyl-d-neuraminic acid
- Gal
d-galactose
- GlcNAc
N-acetyl-d-glucosamine
- Gal-NAc-ol
N-acetyl-d-galactosaminitol
- NMR
nuclear magnetic resonance
- FAB-MS
fast atom bombardmentmass spectrometry 相似文献
5.
Acidic inorganic phosphate (Pi) pool (pH around 6) was detected besides the cytoplasmic pool in intact cells of Chlorella vulgaris 11h by 31P-in vivo nuclear magnetic resonance (NMR) spectroscopy. It was characterized as acidic compartments (vacuoles) in combination with the cytochemical technique; staining the cells with neutral red and chloroquine which are known as basic reagents specifically accumulated in acidic compartments. Under various conditions, the results obtained with the cytochemical methods were well correlated with those obtained from in vivo NMR spectra; the vacuoles were well developed in the cells at the stationary growth phase where the acidic Pi signal was detected. In contrast, cells at the logarithmic phase in which no acidic Pi signal was detected contained only smaller vesicles that accumulated these basic reagents. No acidic compartment was detected by both cytochemical technique and 31P-NMR spectroscopy when the cells were treated with NH4OH. The vacuolar pH was lowered by the anaerobic treatment of the cells in the presence of glucose, while it was not affected by the external pH during the preincubation ranging from 3 to 10. Possible vacuolar functions in unicellular algae especially with respect to intracellular pH regulation are discussed.Non-standard abbreviations EDTA
ethylenediaminetetraacetic acid
- HEPES
N-2-hydroxyethylpiperazine-N-2-ethanesulfonic acid
- MDP
methylene diphosphonic acid
- NMR
nuelear magnetic resonance
- PCA
perchloric acid
- PCV
packed cell volume
- Pi
inorganic phosphate
- Pic
sytoplasmic inorganic phosphate
- Piv
vacuolar inorganic phosphate
- ppm
parts per million
- SP
sugar phosphates
- TCA
trichloroacetic acid 相似文献
6.
Changes in broadline proton nuclear magnetic resonance parameters of cell walls during growth of etiolated hypocotyls of bean (Phaseolus vulgaris L.) indicate that cell wall structure becomes more rigid during development. Most of the changes are completed in the first 6 cm below cotyledon insertion and are correlated with increased restriction of proton movements in regions of dense polymer packing.Abbreviations FID
free induction decay
- M2
second moment
- M2interpair
interpair second moment
- NMR
nuclear magnetic resonance
- T1D
dipolar relaxation time
- T2
spin-spin relaxation time
This work was supported by grants from Natural Sciences and Engineering Research Council of Canada to A.L.M., I.E.P.T. and M. Bloom. 相似文献
7.
Takashi Itoh Hiroshi Funabashi Yoko Katayama-Fujimura Shigeo Iwasaki Hiroshi Kuraishi 《Biochimica et Biophysica Acta (BBA)/General Subjects》1985,840(1):51-55
The structure of methylmenaquinone-7, a major component of methylmenaquinones isolated fromAlteromonas putrefaciens IAM 12079, was determined by comparing the proton nuclear magnetic resonance (1H-NMR) spectrum of its chromenyl derivative with those of menachromenyl acetate prepared from menaquinone-7 and phyllochromenyl acetate. Based on the numbering system used for naphthopyrane nucleus, proton signals of the 7- and 10-position for chromenyl derivatives were assigned from the signals on the1H-NMR spectra phyllochromenyl acetate and phyllochromenol. As a result, the chemical structure of methylmenaquinone-7 was determined as 2,8-dimethyl-3-farnesylgeranygeranyl-1,4-naphthoquinone. 相似文献
8.
The assignment of the 1H nuclear magnetic resonance spectrum of glucagon bound to perdeuterated dodecylphosphocholine micelles with the use of two-dimensional 1H nuclear magnetic resonance techniques at 360 MHz is described. Sequential resonance assignments were obtained for all backbone and Cβ protons except the N-terminal amino group and the amide proton of Ser2. The assignments of the non-labile amino acid side-chain protons are complete except for the γ-methylene protons of Gln20 and Gln24. These assignments provide a basis for the determination of the three-dimensional structure of lipid-bound glucagon. 相似文献
9.
In this study, the antibody 3G9-A was assayed for activity against human erythrocyte glycosphingolipids. The antibody was found to recognize glycosphingolipid components from blood group A erythrocytes but not glycosphingolipids from blood group B or O erythrocytes. Subsequent investigation revealed that the glycosphingolipid components recognized by the antibody were also recognized by a blood group A specific monoclonal antibody. The structures of two of the isolated active glycosphingolipid components were structurally characterized using proteon nuclear magnetic resonance (1H NMR) and gas chromatography-mass spectrometry (GC-MS) techniques and were found to consist of two blood group A glycosphingolipids; the type 2 chain Ab and type 3 chain Aa glycosphingolipids. Subsequent analysis of the remaining active components by GC-MS and immunostaining techniques revealed that all of the active components were blood group A glycosphingolipids. Furthermore, structural studies of the active components suggested that the epitope of the antibody consisted of the group A trisaccharide, GalNAc1,3(Fuc1,2)Gal.Abbreviations GC-MS
gas chromatography-mass spectrometry
-
1H NMR
proton nuclear magnetic resonance
- Gal
d-galactose
- Glc
d-glucose
- Fuc
l-fucose
- GalNAc
N-acetylgalactosamine
- GlcNAc
N-acetylglucosamine
- Cer
ceramide
- mAb
monoclonal antibody
- BSA
bovine serum albumin
- PBS
phosphate buffered saline
- FID
free induction decay
- PMAA
partially methylated alditol acetates 相似文献
10.
Betül Kaya Begüm Nurpelin Sağlık Serkan Levent Zafer Asım Kaplancıklı 《Journal of enzyme inhibition and medicinal chemistry》2016,31(6):1654-1661
In the present work, 12 new 2-(5-substituted-benzothiazol-2-ylsulfanyl)-N-(substitutedbenzyl)-N-(4-substitutedphenyl) acetamide derivatives (4a–l) was designed and synthesized. The structures of the synthesized compounds were clarified using Fourier transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H-NMR), carbon-13 nuclear magnetic resonance (13C-NMR) and high-resolution mass spectrometry (HRMS) spectral data. Purity of synthesized compounds was checked by high-performance liquid chromatography (HPLC) analyses and purity ratio was found between 96.5–99.9%. The inhibitory activity of the compounds against MAO-A and MAO-B enzymes was evaluated by using in vitro flurometric method in which kynuramine was used as a substrate. Most of the compounds exhibited more selective inhibitory activity towards monoamine oxidase B (MAO-B) than monoamine oxidase A (MAO-A). Compound 4h was determined as the most potent compound against both enzyme types. The MAO-B enzyme kinetic of the compound 4h was studied and nature of MAO-B inhibition, caused by this compound, was investigated. The graphical analysis of steady-state inhibition data indicated that compound 4h is a mixed type inhibitor. Theoretical calculation of absorption, distribution, metabolism, excretion (ADME) properties for the synthesized compounds was also carried out and observed data supported the potential of compound 4h. 相似文献
11.
Antonio Evidente Maria Rosaria Cicala Italo Giudicianni Giacomino Randazzo Rodolfo Riccio 《Phytochemistry》1983,22(2):581-584
-The 1H and 13C NMR spectra of lycorine and its α-dihydro derivative have been studied. The employment of nuclear magnetic double resonance, nuclear Overhauser effect and acetylated derivatives, allows the assignment of all proton resonances. The assignments of the carbon shifts have been obtained by means of proton noise decoupled, single frequency off-resonance decoupled, single frequency selective decoupling, time dependence nuclear Overhauser effect and by comparison with reference compounds. 相似文献
12.
Genshiro Kawai Yonosuke Ikeda Keisuke Tubaki 《Bioscience, biotechnology, and biochemistry》2013,77(7):2137-2146
Fruiting bodies were formed around a Penicillium colony which appeared as a contaminant in a culture of Schizophyllum commune, and this phenomenon was reproduced with a synthesized system consisting of S. commune IAM 9006 and P. funiculosum A-l. The active substances were recovered in an acetone extract of the mycelia of P. funiculosum, purified by silica gel column chromatography and reverse-phase high-performance liquid chromatography, and characterized by infrared spectroscopy, gas-liquid chromatography, gas-liquid chromatography-mass spectroscopy and nuclear magnetic resonance spectroscopy. They were ceramides and cerebrosides having nonadecasphingadienine and 2-hydroxy fatty acid moieties in common. The major component was identified as (4E,8E)-N-2′-hydroxy-(E)-3′-octadecenoyl-1-O-β-glucopyranosyl-9-methyl-4,8-sphingadienine. 相似文献
13.
Summary Developing pea (Pisum sativum L.) seeds were chosen to evaluate the performance of various nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) methods of detecting sucrose in plants. The methods included chemical shift selective imaging (CHESS), heteronuclear correlation via13C-1H coupling (HMQC), and homonuclear correlation via1H-1H coupling (DQF). The same experiments were also performed on sucrose phantom samples to evaluate the methods in the absence of the line broadening observed in plant systems. Using the spin echo technique for multi-slice imaging, we could discern the detailed internal structure of the intact seed with a resolution of tens of microns. The proton spin-lattice relaxation time and linewidth as a function of the age of the seed were measured to optimize the efficiency of the NMR and MR experiments. The age-dependent changes in these NMR parameters are consistent with the accumulation of insoluble starch as age increases. Both the NMR and MRI results are in accord with the results of chemical analysis, which reveal that the sucrose concentration is higher in the embryo than in the seed coat, and glucose is at low concentration throughout the seed. Of the three methods for proton observation, the enhanced version of the CHESS approach (CD-CHESS) provides the best combination of sucrose detection and water suppression. Direct observation of13C is preferable to indirect detection using HMQC because of water signal bleed-through in samples with large (>200 Hz) linewidths.Abbreviations CD-CHESS
continuous wave decoupling chemical shift selective imaging
- CHESS
chemical shift selective imaging
- CSI
chemical shift imaging
- CW
continuous wave
- DQF
homonuclear double quantum filtering
- FOV
field of view
- FW
fresh weight
- GHMQC
gradient version of the heteronuclear multiple quantum coherence 相似文献
14.
High resolution proton nuclear magnetic resonance has been used to observe protons at the active site of chymotrypsin Aδ and at the same region of chymotrypsinogen A. A single resonance with the intensity of one proton is located in the low field region of the nuclear magnetic resonance spectrum. This resonance is observed in H2O solutions but not in 2H2O. On going from low to high pH the resonance titrates upfield 3 parts per million in both proteins and has a pK of 7.5. The titration can be prevented by alkylating His57 with either of two active site directed chloromethyl ketones. Using these data the proton resonance has been assigned to a proton in a hydrogen bond between His57 and Asp102. Further confirmation of this assignment lies in the observation of a similar resonance in this same low field region of the nuclear magnetic resonance spectrum of trypsin, trypsinogen, subtilisin BPN′ and α-lytic protease all of which have the Asp-His-Ser triad at their active sites.This proton resonance in chymotrypsin Aδ was used as a probe to monitor the charge state of the active site upon formation of a stable acyl-enzyme analogue N2(N-acetylalanyl)-N1benzoylcarbazoyl-chymotrypsin Aδ. In this derivative the His-Asp proton resonance titrates from the same low pH end point as in the native enzyme, ?18 parts per million, to a new high pH end point of ?14.4 parts per million (versus ?15.0 parts per million in the native enzyme). The difference of 0.6 parts per million in the high pH end points between the native and acyl enzyme is interpreted as supporting the suggestion that a hydrogen bond exists between Ser195 and His57 in the native enzyme and zymogen.We conclude from these studies that the charge relay system from Asp102 across His57 to Ser195 is intact in chymotrypsin Aδ and chymotrypsinogen A, and that, in the native enzyme, it slightly polarizes Ser195. 相似文献
15.
T. Asakura K. Adachi J.S. wiley L.W.-M. Fung C. Ho J.V. Kilmartin M.F. Perutz 《Journal of molecular biology》1976,104(1):185-195
We have purified haemoglobin Philly by isoelectric focusing on polyacrylamide gel, and studied its oxygen equilibrium, proton nuclear magnetic resonance spectra, mechanical stability, and pH-dependent u.v. difference spectrum. Stripped haemoglobin Philly binds oxygen non-co-operatively with high affinity. Inorganic phosphate and 2,3-diphosphoglycerate have little effect on the equilibrium curve, but inositol hexaphosphate lowers the affinity and induces co-operativity. These properties are explained by the nuclear magnetic resonance spectra which show that stripped deoxyhaemoglobin Philly has the quaternary oxy structure and that inositol hexaphosphate converts it to the deoxy structure. An exchangeable proton resonance at ?8.3 p.p.m. from water, which is present in oxy- and deoxyhaemoglobin A, is absent in both these derivatives of haemoglobin Philly and can therefore be assigned to one of the hydrogen bonds made by tyrosine C1-(35)β, probably the one to aspartate H8(126)α at the α1β1 contact. Haemoglobin Philly shows the same pH-dependent u.v. difference spectrum as haemoglobin A, only weaker, so that a tyrosine other than 35β must be mainly responsible for this. 相似文献
16.
The helix–coil transition of poly-N5-(3-hydroxypropyl)-L -glutamine in methanol–water solutions has been observed using 13C nuclear magnetic resonance. Two signals appear in the α-CH region in the course of the transition; this is in contrast with previous proton magnetic resonance experiments carried out on this polymer in the same solvent system. 相似文献
17.
Incubation of sections of various tissues of Pinus pinea L. with a relatively low concentration (3.6 μM) of indole-3-acetic acid-2-14C (IAA) resulted in the formation of two major metabolites. The first, which has not been identified, seemed to be a polar acidic compound and the second was identified as indole-3-acetylaspartic acid (IAAsp). The polar acidic metabolite has been found to be the major metabolite in needles, shoot wood and roots, while IAAsp has been found to be the major metabolite in shoot bark. Increasing the concentration of IAA in the incubation medium resulted in an increase in the formation of a third metabolite which proved to be l-O-(indole-3-acetyl)-β-d -glucose (IAGlu) and a concomitant decrease in the amount of the polar acidic metabolite. This phenomenon was prominent particularly in needles. IAGlu was isolated from needles and IAAsp was isolated from shoot bark by means of polyvinylpolypyrrolidone column chromatography and preparative thin-layer chromatography. IAGlu was identified by comparison with authentic material by co-chromatography in three different solvent systems and by 1H-nuclear magnetic resonance analysis. IAAsp was identified by comparison with authentic material by gas-liquid chromatography and 1H-nuclear magnetic resonance analysis. Several aspects of formation, separation and isolation of IAA metabolites are discussed. 相似文献
18.
Noriko Takahashi Tsukasa Matsuda Kazuno Shikami Ichio Shimada Yoji Arata Ryo Nakamura 《Glycoconjugate journal》1993,10(6):425-434
Asparagine-linked oligosaccharides of duck ovomucoid were released quantitatively from the protein by digestion with glycoamidase A (from almond), the reducing ends of the oligosaccharide chains thus obtained were aminated with a fluorescent reagent, 2-aminopyridine, and the mixture of pyridylamino derivatives of the oligosaccharides was separated using two different types of high performance liquid chromatography (HPLC) on a reversed phase column and an amide adsorption column. More than sixteen different oligosaccharides were separated and the structures were characterized by a combination of the 2-dimensional sugar mapping technique using HPLC, exoglycosidase digestion, and proton nuclear magnetic resonance measurements (1- and 2-dimensional). Furthermore, the HPLC profile of duck ovomucoid oligosaccharides was compared with previously reported profiles obtained from quail and chicken ovomucoids.Abbreviations COSY
chemical shift-correlated spectroscopy
- DQF-COSY
double quantum filtered COSY
- DSS
sodium, 4,4-dimethyl-4-silapentane 1-sulfonate
- Gal
D-galactose
- GlcNAc or GN
N-acetyl-D-glucosamine
- HOHAHA
homonuclear Hartmann-Hahn spectroscopy
- Man or M
D-mannose
- NOE
nuclear Overhauser enhancement
- ODS
octadecylsilyl
- PA
pyridylamino
- ROESY
rotating frame nuclear Overhauser effect spectroscopy
- SDS/PAGE
sodium dodecyl sulfate/polyacrylamide gel electrophoresis 相似文献
19.
Lihong Shan Kai Jiao Minghui Yin Jiajia Huang Yanjie Chen 《Biocatalysis and Biotransformation》2016,34(3):83-88
In this work, we report the mode of biotransformation of 5-en-3β-ol steroids using Mucor circinelloides lusitanicus for the first time. Here, we selected seven 5-en-3β-ol steroids as substrates. The main characteristic of the fungus was to introduce a 7α-hydroxyl group into substrates 1--5. With substrate 2, 3β, 7α, 11α-trihydroxypregna-5-en-20-one (2b) was obtained as the final product in good yield (46.4%). All the metabolites were determined by infrared spectra, high-resolution mass spectrometry, proton nuclear magnetic resonance, and carbon-13 nuclear magnetic resonance. 相似文献
20.
Several molecules like ionophores, vitamins, ion-binding cyclic peptides, acidic phospholipids, surfactants are known to expose
the inner side of vesicles, to the externally added cations. Whereas ionophores and certain other systems bring about these
changes by a selective transport (influx) of the cation by specialized mechanisms known as the carrier and channel mechanism,
other systems cause lysis and vesicle fusion. These systems have been successfully studied using1H,31 P and13C nuclear magnetic resonance spectroscopy after the demonstration, fifteen years ago, of the ability of paramagnetic lanthanide
ions to distinguish the inside of the vesicle from the outside. The results of these ’nuclear magnetic resonance kinetics’
experiments are reviewed. 相似文献