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1.
In the current investigation complexation of the gemifloxacin (GIN) with technetium-99 m (99mTc) and its biological evaluation in artificially Streptococcus pneumoniae (S. pneumoniae) infected rats was assessed as potential S. pneumoniae infection radiotracer. Radiochemically the 99mTc-GIN complex was further analyzed in terms of stability in saline, in vitro stability in serum at 37 °C, in vitro binding with S. pneumoniae and biodistribution in artificially S. pneumoniae (living and heat killed) infected rats. The complex was found 97.25 ± 0.25% radiochemically stable in saline at 30 min after reconstitution. The stability of the 99mTc-GIN complex was decreased to 90.50 ± 0.20% within 240 min after reconstitution. In serum the 99mTc-GIN complex showed stable profile with the appearance of 18.85% free tracer within 16 h of incubation. The 99mTc-GIN complex showed saturated in vitro binding with S. pneumoniae after different intervals. Almost five fold uptake was observed in living S. pneumoniae infected muscle of the rats as compared to the inflamed and normal muscle. No significant difference in the uptake of heat killed S. pneumoniae infected, inflamed and normal muscles of the rats. The high RCP yield in saline, in vitro permanence in serum, in vitro binding with living S. pneumoniae and biodistribution in artificially S. pneumoniae infected rats we recommend the 99mTc-GIN as potential S. pneumoniae infection radiotracer.  相似文献   

2.
A novel cyclopropane derivative, 1-cyano-N-p-tolylcyclopropanecarboxamide (C12H12N2O, Mr = 200.24) was synthesized and its structure was studied by X-ray diffraction, FTIR, 1H and 13C NMR spectrum and MS. The crystals are monoclinic, space group P2_1/c with a = 7.109 (4), b = 13.758 (7), c = 11.505 (6) Å, α = 90.00, β = 102.731 (8), γ = 90.00 °, V = 1097.6 (9) Å3, Z = 4, F(000) = 312, D c  = 1.212 g/cm3, μ = 0.0800 mm?1, the final R = 0.0490 and wR = 0.1480 for 1,375 observed reflections with I > 2σ(I). A total of 6,109 reflections were collected, of which 2,290 were independent (R int = 0.0290). Theoretical calculation of the title compound was carried out with HF/6-31G (d,p), B3LYP/6-31G (d,p), MP2/6-31G (d,p). The full geometry optimization was carried out using 6-31G(d,p) basis set, and the frontier orbital energy. Atomic net charges were discussed, and the structure-activity relationship was also studied. The preliminary biological test showed that the synthesized compound is bioactive against the KARI of Escherichia coli.  相似文献   

3.
Two thiosemicarbazones, (E)-2-(2,4-dimethoxybenzylidene)thiosemicarbazone (24-MBTSC (1)) and (E)-2-(2,5-dimethoxybenzylidene)thiosemicarbazone (25-MBTSC (2)), derived from 2,4-dimethoxybenzaldehyde and 2,5-dimethoxybenzaldehyde, respectively, with thiosemicarbazide have been synthesized and their structures were characterized by elemental analyses, FT-IR, 1H NMR spectroscopy, and X-ray single-crystal diffraction analysis. Molecular orbital calculations have been carried out for 1 and 2 by using an ab initio method (HF) and also density functional method (B3LYP) at 6-31G basis set. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.1342(5) Å, b = 18.1406(10) Å, c = 8.2847(6) Å, β = 109.7258(17)°, V = 1150.75(12) Å3, and Z = 4, whereas compound 2 crystallizes in the orthorhombic system, space group Pbca, with a = 11.0868(6) Å, b = 13.1332(6) Å, c = 15.9006(8) Å, V = 2315.2(2) Å3, and Z = 8. The compounds 1 and 2 displays a trans-configuration about the C=N double bond.  相似文献   

4.
The present investigation aimed to study and compare the efficiency of non-viable fungal isolates to remove divalent lead (Pb(II)) from aqueous streams. The selected fungal isolates showed identity with Aspergillus caespitosus, Aureobasidium sp. RBSS-303 and Aspergillus flavus HF5 as confirmed using gene sequencing of ITS regions of the ribosomal DNA (rDNA). The obtained equilibrium data for Pb(II) biosorption of A. caespitosus fitted better to Langmuir isotherm with maximum sorption capacity of 351.0 mg/g and A. sp. RBSS-303 and A. flavus HF5 showed good fit to Freundlich isotherm with maximum sorption capacity of 271.5 and 346.3 mg/g respectively. The values of thermodynamic factors ascertained the nature of adsorption process is endothermic with A. caespitosus and A. flavus HF5 but exothermic with A. sp. RBSS-303. The experimental data for Pb(II) biosorption fits very well to pseudo second order kinetic model. With HCl the maximum 85.5, 75.3, 73.7% recovery of Pb(II) was obtained from A. caespitosus, A. sp. RBSS-303 and A. flavus HF5, respectively. The observed percentage loss in sorption capacity of Pb(II) was 3.9% by A. flavus HF5, 12.2% by A. caespitosus and 26.6% by A. sp. RBSS-303 after five cyclic studies of sorption and desorption. Results from the study confirmed the efficiency order of A. caespitosus > A. flavus HF5 > A. sp. RBSS-303 to remove and recover Pb(II) from aqueous solution. Finally, the fungal biosorbents can be used as soil conditioning agent after compositing into valuables fungal protein.  相似文献   

5.
Chemical preparation, crystal structure, and NMR spectroscopy of a new trans-2,5-dimethylpiperazinium monophosphate are given. This new compound crystallizes in the triclinic system, with the space group P-1 and the following parameters: a = 6.5033(3), b = 7.6942(4), c = 8.1473(5) Å, α = 114.997(3), β = 92.341(3), γ = 113.136(3), V = 329.14(3) Å3, Z = 1, and Dx = 1.565 g cm?3. The crystal structure has been determined and refined to R = 0.030 and R w(F 2) = 0.032 using 1558 independent reflections. The structure can be described as infinite [H2PO4] n n? chains with (C6H16N2)2+ organic cations anchored between adjacent polyanions to form columns of anions and cations running along the b axis. This compound has also been investigated by IR, thermal, and solid-state, 13C and 31P MAS NMR spectroscopies and Ab initio calculations.  相似文献   

6.
A stability-indicating UPLC method was developed for quantitative determination of 9-desmethyl-α-dihydrotetrabenazine (9-DM-α-DTBZ), the precursor for preparing a widely used vesicular monoamine transporter 2 imaging agent 11C-α-DTBZ. Compound 9-DM-α-DTBZ was subjected to various stress conditions consisting of acidic, alkaline, oxidative, thermal and photolytic forced degradation. The decomposition of 9-DM-α-DTBZ was observed under oxidative condition, whereas no obvious degradation was shown under the other stress conditions. For chromatographic separation of 9-DM-α-DTBZ and its degradation products, an Acquity UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) and a mobile phase of 20:80 (v/v) methanol/ammonium acetate buffer (pH 4.5, 10 mM) were used. Quantitative determination of 9-DM-α-DTBZ was performed using a PDA detector at a flow rate of 0.30 mL min?1. UPLC–MS analysis was further utilized to characterize the two degradation products. The proposed method was fully validated as per USP guidelines with respect to linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The linear regression analysis showed a good linear relationship (r 2  = 0.9995) in the concentration range of 0.001–1.00 mg mL?1 (n = 6). The assay method was found to have good precision (1.14–1.35% RSD) and recovery (98.91–101.23%). Additionally, the LOD and LOQ of 9-DM-α-DTBZ were 0.30 and 1.00 μg mL?1, respectively. These results indicated that the present method could be used to evaluate the quality of regular production samples and also used in stability assays.  相似文献   

7.
A new metal–organic compound FeF6(HAmTAZ)3 which (HAmTAZ = 3-amino-1,2,4-triazole) was hydrothermally synthesized from an equimolar mixture of FeF2 and FeF3 with HAmTAZ, aqueous HF and ethanol solvent at 410 K yielded a new hybrid class I fluoroferrate. The structure was characterized by single-crystal X-ray diffraction data. The crystal structure of FeF6(HAmTAZ)3 crystallizes in the trigonal system space group R3c with a = b = 12.5230 (6) Å, c = 18.5950 (16) Å, γ = 120° and Z = 6. The structure was built up from isolated octahedral FeF6 separated by [HAmTAZ]+ cations. The thermal analysis has shown that the decomposition undergoes two steps between 475 and 775 K. IR and mass spectrometry have been used to confirm the presence of the organic molecule in the crystal lattice and determine the evacuated vapours during the decomposition, respectively. The magnetization of the title compound has no revealed any ferromagnetic component in the range of magnetic field from ?20 to 20 KOe at room temperature.  相似文献   

8.
The molecular and crystal structures of the title compound, C16H18N2O, were characterized and determined by single crystal X-ray diffraction method in addition to spectroscopic means such as IR, UV–VIS and 1H NMR. The compound crystallizes in orthorhombic space group P bca, with a = 9.3350(5) Å, b = 23.4878(13) Å, c = 26.5871(12) Å, Z = 16, D calc. = 1.1591(1) g/cm3, μ (MoKα) = 0.073 mm?1. Monomers of the compound in the crystal structure are linked into C(7) and C(8) chains generated by translation along the [1 0 0] direction with the aid of O–H···N type H-bonds which serve to the stabilization of periodic organization of the molecules beside major and minor component in the disordered azo fragment. In order to describe conformational flexibility and the crystal packing effects on the molecular conformation, potential barriers regarding the rotation along both Ar–N bonds were calculated by varying the related torsional degrees of freedom in every 10° ranging from ?180° to +180° via quantum chemical calculations at DFT/B3LYP level.  相似文献   

9.
A new Cu(II) complex, [Cu2(bzpy)2(Hbpd)2(H2O)](ClO4)2·H2O (1) based on bzpy (bzpy = 2-benzoylpyridine) and H2bpd (benzyl-2-pyridylmethanediol) mixing ligands, was synthesized and characterized by IR, UV–Vis spectra, TGA and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P2(1)/n with a = 18.7790(2), b = 14.4609(3), c = 18.9434(4) Å, β = 102.17°, V = 5028.63(16) Å3, Z = 4. The complex bears a dinuclear structure in which two Cu(II) atoms adopt elongated square pyramidal (SP) and octahedral geometry, respectively, and two intramolecular π…π interactions are also observed. Then with the help of intermolecular π…π and CH…π interactions, a 1D chain structure is formed based on the dinuclear unit. Thermal stability of 1 was studied.  相似文献   

10.
Oxidative stress induced by oxygen free radicals (OFRs) is a casual factor in psoriasis. Our aim was to detect the oxidative stress parameters and blood plasma changes with differential scanning calorimetry (DSC) in psoriatic patients. The study included untreated (n = 39) and treated (retinoids, methotrexate, biologic response modifiers; n = 33) white adult patients from both sex. To monitor oxidative stress concentration of malondialdehyde (MDA), reduced glutathione and sulfhydryl groups, production of OFRs, and activity of myeloperoxidase (MPO), superoxide dismutase, and catalase were measured. Denaturation of plasma components was detected in SETARAM Micro DSC-II calorimeter. Total production of OFRs and MPO activity, and the concentration of MDA were significantly increased both in untreated patients with moderate and severe symptoms and in all drug-treated groups compared with controls (p < 0.001). All of the scavengers and antioxidants were significantly decreased in untreated patients and better preserved after retinoid and biological therapy. DSC scans of blood plasma showed melting temperature a characteristic parameter to follow the severity of disease. The calorimetric enthalpy is exhibiting a moderate decrease with the progression of the inflammation. These findings suggest that an imbalance exists between pro-oxidants and antioxidants in untreated severe psoriatic patients. All drug therapy reduced the changes, mainly the biologic response modifiers. Similarly, DSC showed differences between untreated and conventional systemic drug treatment.  相似文献   

11.
We report a detailed comparison between RF and microwave (HF) plasmas of N2 and Ar–20 %N2 as well as in the corresponding afterglows by comparing densities of active species at nearly the same discharge conditions of tube diameter (5–6 mm), gas pressure (6–8 Torr), flow rate (0.6–1.0 slm) and applied power (50–150 W). The analysis reveals an interesting difference between the two cases; the length of the RF plasma (~25 cm) is measured to be much longer than that of HF (6 cm). This ensures a much longer residence time (10?2 s) of the active species in the N2 RF plasma [compared to that (10?3 s) of HF], providing a condition for an efficient vibrational excitation of N2(X, v) by (V–V) climbing-up processes, making the RF plasma more vibrationally excited than the HF one. As a result of high V–V plasma excitation in RF, the densities of the vibrationally excited N2(X, v > 13) molecules are higher in the RF afterglow than in the HF afterglow. Destruction of N2(X, v) due to the tube wall is estimated to be very similar between the two system as can be inferred from the γv destruction probability of N2(X, v > 3–13) on the tube wall (2–3 × 10?3 for both cases) obtained from a comparison between the density of N2(X, v > 3–9) in the plasmas to that of the N2(X, v > 13) in the long afterglows. Interestingly enough, densities of N-atoms and N2(A) metastable molecules in the afterglow regions, however, are measured to be very similar with each other. The measured lower density of N2 + ions than expected in the HF afterglow is rationalized from a high oxygen impurity in our HF setup since N2 + ions are very sensitive to oxygen impurity .  相似文献   

12.
Fourier transform infrared (FTIR) spectroscopy studies were performed to confirm and to provide information on the identity and binding characteristics of the chemical groups responsible for the binding of elements using Aspergillus niger (A. niger) wild-type strains. Two absorption bands in the 3690–3615 and 2970–2895 cm?1 regions can characterize stretching vibrations OH and CH groups in fatty acids, respectively, and intensive bands around of 1600 cm?1 and by 1048 cm?1 correspond to stretching vibrations of C=O groups of amides (amide I) or stretching vibrations ν(C–N). The FTIR results confirmed that no extra differences between IR spectra of A. niger in raw biomass and in solid rest after extraction with chloroform were observed. The small differences were observed in IR spectra of A. niger in chloroform after extraction.  相似文献   

13.
A gradient-specific stability indicating HPLC method was developed and validated for the determination of the antidiabetic agent anagliptin in laboratory mixtures. Reversed-phase chromatography was performed using a Shimadzu LC-20 AD pump (binary), Shimadzu PDA M-20A diode array detector, and Waters Symmetry C-18 column (150?×?4.6 mm, 3.5 µm) maintained at a column oven temperature of 40 °C with UV detection at 247 nm. A gradient program was run at flow rate of 1 mL min?1. Mobile phase A consisted of a mixture of acetate buffer(10 mm) pH 5/methanol/acetonitrile in the ratio of 90:5:5. Mobile phase B consisted of a mixture of acetate buffer (10 mm) pH 5/methanol/acetonitrile in the ratio of 50:25:25. The method was validated according International Conference of Harmonization (ICH) guidelines. Linearity was observed in the concentration range of 10–120 µg/mL with regression coefficient r2(0.999). The LOD was found to be 7.8 µg/mL and LOQ was found to be 22.68 µg/mL. Anagliptin was subjected to stresses such as acidic, alkali, oxidation, photolysis, and thermal conditions. The proposed method was validated as per ICH guidelines and was found to be accurate, precise, and specific. The drug showed significant degradation in alkaline and oxidative conditions. Alkaline and oxidative degradation followed first-order kinetics. Degradation rate constant and half-lives were determined. Degradation products in alkaline and oxidative conditions were identified by LC–MS. One major degradation product was isolated from each condition by preparative HPLC. These degradation products were characterized by 1H NMR, 13C NMR, DEPT, D2O exchange, MS/MS, HRMS, and IR techniques. From the spectral data the alkaline degradation product was characterized as 1-{2-[1-(2-methylpyrazolo[1,5-a]pyrimidine-6-carboxamido)-methyl-propan-2-yl-amino]acetyl}pyrrolidine-2-carboxamide. The oxidative degradation product was characterized as N-[2-({2-[(2S)-2-cyanopyrrolidin-1-yl]-2-oxoethyl}amino)-2-methylpropyl]-2-methylpyrazolo-[1,5-a]pyrimidine-N-oxido-6-carboxamide.  相似文献   

14.
The first inorg/organic hybrid complex incorporating the macrocyclic oxamide, of formula [(NiL)2Cu2(μ-NSC)2(NSC)2] (1), (NiL, H2L = 2, 3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-dien), have been synthesized and structurally characterized. The crystals crystallize in the triclinic system, space group P-1, for (1) a = 8.319(3) Å, b = 10.434(4) Å, c = 14.166(5) Å, a = 107.030(5)°, β  =  91.257(5)°, γ = 107.623(5)°. The complex involved both bridging N, S-ligand, and oxamide ligand, C–H?S interactions and NCS → Ni weak coordination interactions making the complex superamolecular.  相似文献   

15.
A simple, rapid, and sensitive non-aqueous capillary electrophoresis procedure for the quantitative determination of matrine and oxymatrine is established. Optimum separation conditions were obtained when the sample was injected under pressure for 3 s at 50 mbar and separated with the buffer containing 70 mM ammonium acetate, 7.0% (v/v) acetic acid, and 10% (v/v) acetonitrile in methanol medium at 25 kV applied voltage. The analytes were detected at 205 nm. The two alkaloids can be separated within 12 min and quantified with high sensitivity. The method was validated in terms of reproducibility, linearity, and accuracy when applied to the analysis of matrine and oxymatrine in Sophora flavescens and its medicinal preparations.  相似文献   

16.
Recombinant Escherichia coli cells harboring nitrilase from Alcaligenes faecalis were immobilized using tris(hydroxymethyl)phosphine (THP) as the coupling agent. The optimal pH and temperature of the THP-immobilized cells were determined at pH 8.0 and 55 °C. The half-lives of THP-immobilized cells measured at 35, 40, and 50 °C were 1800, 965, and 163 h, respectively. The concentration of R-mandelic acid (R-MA) reached 358 mM after merely 1-h conversion by the immobilized cells with 500 mM R,S-mandelonitrile (R,S-MN), affording the highest productivity of 1307 g L?1 day?1 and the space-time productivity of 143.2 mmol L?1 h?1 g?1. The immobilized cells with granular shape were successfully recycled for 60 batches using 100 mM R,S-MN as substrate at 40 °C with 64% of relative activity, suggesting that the immobilized E. coli cells obtained in this study are promising for the production of R-MA.  相似文献   

17.
The potential-energy surface for the Li(2S)–HF (? X1Σ+ interaction, where HF is kept rigid, is calculated using the supermolecular unrestricted fourth-order Møller–Plesset perturbation theory. The basis set superposition error corrected potential indicates two minima. The global minimum occurs for the bent Li...FH structure at R=1.95 Å and θ=70° with a relatively deep well of De=1,706 cm?1 and the secondary minimum is found for the linear Li...HF configuration at R=4.11 Å with a well depth ofDe=288 cm?1. A barrier of 177 cm?1 (with respect to the secondary linear minimum) separates these two minima. In this study 27 bound states of the bent Li...FH minimum and eight bound states of the linear Li...HF minimum up to the Li+HF dissociation threshold are calculated. The energy partitioning using the intermolecular perturbation theory scheme shows that the origins of the stability of the structures studied are entirely different. The global minimum is stabilised using the attractive Coulombic interaction and unrestricted Hartree–Fock deformation energy. The latter term originates from the mutual electric polarisation effects. The secondary linear minimum is mostly determined by the anisotropy of the repulsive Heitler–London exchange-penetration and attractive dispersion energies.  相似文献   

18.
In a majority of environments, microbes live as interacting communities. Microbial communities are composed of a mix of microbes with often unknown functions. Polymicrobial diseases represent the clinical and pathological manifestations induced by the presence of multiple infectious agents. These diseases are difficult to diagnose and treat and usually are more severe than monomicrobial infections. The interaction relationship between Enterococcus faecalis and Escherichia coli was researched using a Calvet calorimeter. Three mixtures of both bacteria were prepared in the following proportions: 20 + 80 % (0.2 mL E. faecalis + 0.8 mL E. coli), 50 + 50 % (0.5 mL E. faecalis + 0.5 mL E. coli) and 80 + 20 % (0.8 mL E. faecalis + 0.2 mL E. coli). Experiments were carried out at concentration of 106 CFU mL?1 and a constant temperature of 309.65 K. The differences in shape of graph of E. faecalis, E. coli and their mixtures were compared. Also, the thermokinetic parameters such as detection time (t d), growth constant (k), generation time (G) and the amount of heat released (Q) were calculated.  相似文献   

19.
Cu(II) complexes of the tridentate ligand N-(methylpyridin-2-yl)-amidino-O-methylurea (L), namely [Cu(L)Cl2] and [Cu(L)ClO4]ClO4, have been investigated for interactions with DNA by spectroscopic methods and viscosity measurements. Both complexes bind to DNA through non-intercalative interactions. [Cu(L)Cl2] (K b = 2.81 × 105 M?1) shows similar DNA-binding potential to [Cu(L)ClO4]ClO4 (K b = 1.57 × 105 M?1). Investigation of the chemical nuclease properties toward plasmid pBR322 DNA by gel electrophoresis and atomic force microscopy (AFM) suggests that both complexes are able to cleave the supercoiled form (Form I) to the nicked (Form II) and linear forms (Form III) through an oxidative pathway. The possible reactive oxygen species have been investigated by the use of scavengers, indicating that hydroxyl radicals may be involved in the DNA cleavage mechanism. Both of these complexes show similar activities against selected human cancer cell lines.  相似文献   

20.
For the first time in the published literature, a study is described concerning the use of the saw-sedge Cladium mariscus (C. mariscus) for adsorption of 2,4-dichlorophenoxyacetic acid (2,4-D) from aqueous systems. Among the experiments carried out, the elemental composition of C. mariscus was determined (C = 48.0 %, H = 7.1 %, N = 0.95 %, S = 0.4 %), FTIR spectroscopic analysis was performed to confirm the chemical structure of the adsorbent, and porous structure parameters were measured: BET surface area (A BET  = 0.6 m2/g), total pore volume (V p  = 0.001 cm3/g) and average pore size (S p  = 6.6 nm). It was shown that the effectiveness of removal of 2,4-D from aqueous systems using C. mariscus depends on parameters of the process: contact time, system pH, mass of sorbent, and temperature. Maximum adsorption was attained for a solution at pH = 3. Further increase in the alkalinity of the tested systems led to a reduction in the effectiveness of the process. The kinetic of adsorption of 2,4-D by C. mariscus was also determined, and thermodynamic aspects were investigated. The experimental data obtained correspond to a pseudo-second-order kinetic model of type 1. Additionally the negative values obtained for ΔHº indicate that the process is exothermic, and the negative values of ΔGº show it to be spontaneous. As the temperature of the system increases the spontaneity of adsorption is reduced, in accordance with the exothermic nature of the process.  相似文献   

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