Study of spatial distribution for the active ingredient in ibuprofen tablet based on near-infrared micro-imaging technology

The NIR micro-images of ibuprofen tablets were collected in this research.Compare correlation imaging and principal component analysis(PC A) with histogram were applied to acquire the spatial distribution of ibuprofen granule.The result indicated that a similar distribution trend can be acquired by both of the two methods mentioned above;the information of PC2 results from ibuprofen mainly since the correlation coefficient between PC2 loading vector and the NIR spectrum of ibuprofen is 0.9930.The result of PCA indicated that the information of PC2 results from ibuprofen mainly for both the low and the high content of ibuprofen in the tablets.The correlation coefficient between the data of the two PC2 loading vectors of the low and the high content of ibuprofen in the tablets is 0.9998,which indicates that the result of PCA is stable and reliable.     

Two Typical Examples of Scaling Ionic Partition Scheme for Estimating Correlation Energy of A2 Type Molecules

Based on the calculation results of pair correlation energy contributions of the various electron pairs in Na2 and H2NNH2 systems and the application of the scaling ionic partition scheme for symmetrical A2 type systems, the total correlation energies of Na2 and H2NNH2 have been reproduced by using this simple scheme. The two results show that the absolute deviations are within an acceptable range of error, however, in this way, more than 90% of computational work can be saved. The most attractive result in present paper is that, in these two molecules the coefficients c1 and c2 in the estimation equation can be obtained by the proportion of correlation energy of A^- to that of A^ singlet system. Therefore, it is believed that the proposed ionic partition scheme for symmetrical A2 molecules would be very useful to estimate the correlation energies of large symmetrical molecules.     

Interactions of acetylcholinesterase with salvianolic acid B and rosmarinic acid from Salvia miltiorhiza water extract investigated by NMR relaxation rate

In order to understand whether the ameliorating effect on old ages memory disorder by the root of Salvia miltiorhiza is related to the acetylcholinesterase （ACHE） inhibition, two main ingredients, salvianolic acid B （1） and rosmarinic acid （2）, which were isolated from S. miltiorhiza water extract, were investigated in vitro by NMR relaxation rate in this work. The results showed that the proton selective relaxation rates and the molecular rotational correlation time of proton pairs for compounds 1 and 2 increased significantly by adding of AChE in mixing solution. The study reveals that the two compounds might bind to the enzyme and have ACHE inhibitory effect, which could contribute to the ameliorating effect at some extent on old ages memory disorder.     

The structural analysis of the inclusion complex of β-cyclodextrin with m-nitrophenoxyacetic acid

The inclusion complex of β-cyclodextrin with m-nitrophenoxyacetic acid was studied by single crystal X-ray diffraction,2D NMR spectroscopy and semi-empirical methods AMI.The crystallographic study shows that two β-cyclodextrins are held together by hydrogen bonds to form head-to-head dimers.The disordered guest molecule adjusts itself to attain the most stable accommodation into the cavity in which the nitro group is located at the dimer interface while the carboxyl group is buried in the primary hydroxyl groups of β-cyclodextrin.The guest inside the cavity is disordered over two sites and exhibits mobility.Moreover,2D NMR spectroscopy and theoretical study show the same inclusion behavior.In comparison to the inclusion complex of β-cyclodextrin with p-nitrophenoxyacetic acid,the host-guest stoichiometries are different,i.e.,2:1 for m-nitrophenoxyacetic acid and 1:1 for p-nitrophenoxyacetic acid,while the inclusion orientation and the packing pattern of the host are similar in both complexes.     

Dispersion state of CuO on CeO_2——An incorporation model for the interaction between metal oxide and oxide support

XRD and XPS are used to study the dispersion state of CuO on ceria surface.The dispersion capacity values of CuO measured by the two methods are consistent,which are of 1.20 mmol CuO/100 m CeO2.In addition,the results reveal that highly dispersed Cu2 + ions are formed at low CuO loadings and that increasing the CuO content to a value higher than its dispersion capacity produces crystalline CuO after the surface vacant sites on CeO2 are filled.The atomic composition of the outermost layer of the CuO/CeO2 samples has been probed by using static secondary ion mass spectroscopy (SSIMS),and the ratios of Cu/Ce are found to be 0.93 and 0.46 for the 1.22 and 0 61 mmol CuO/CeO2 samples respectively.Temperature-programmed reduction (TPR) profile with two reduction peaks at 156 and 16513 suggests that the reduction of highly dispersed Cu2+ ions consists of two steps and is easier than that of CuO crystallites,in which the TPR profile has only one reduction peak at about 249℃.The above experimental results are in     

Synthesis and characterization of a new catalyst for RhB degradation constructed by [SiMo12O40]4- anionic cluster

A Keggin-type polyoxomolybdate[H_2biim]{Ni(biim)_3(SiMO_(12)O_(40))}[biim =1H,1'H-[2,2']biimidazolyl]has been synthesized under hydrothermal condition and characterized by XRD,temperature-dependent IR,TG,temperature-induced and magnetism-induced 2D infrared correlation spectroscopy(2D-IR COS)and UV-vis DRS in order to explore the relationship between structure and properties.Temperatureinduced 2D-IR COS spectroscopy indicates that the terminal Mo-O_(μ/υ) bonds are more sensitive than the bridging Mo=O_t,bands to temperature variation,which is in agreement with the conclusion of temperature-dependent IR.Magnetism-dependent 2D-IR COS spectroscopy reveals the stretching vibration of the Mo=O_t,occurs prior to the stretching vibration of the Mo-O_(μ/υ),which is due to the coordination environment and the valence of the Si atom.The stability of compound 1 is investigated via TG and temperature-dependent IR.In RhB degradation,compound 1 shows good photocatalytic abilities.     

Spectroscopic Study on Interaction of β-Cyclodextrin with Triprolidine Hydrochloride

The complexation of triprolidine hydrochloride （TRP） and β-cyclodextrin （β-CD） in deuterium oxide was investigated by 400 MHz 1^H NMR spectroscopy. The 800 MHz 2D ROESY data revealed that two 1 ：1 and one 2 ： 1 β-CD-TRP inclusion complexes were formed. Both aromatic moieties （p-tolyl and pyridyl ring） has entered into the β-CD cavity, confirming the existence of two different equilibria for 1 ： 1 inclusion complexes in which p-tolyl ring of the guest is more tightly held by the host cavity. The ROE intermolecular interactions provided the plausible structures of these 1 ： 1 and 2 ： 1 stoichiometric inclusion complexes of β-CD-triprolidine hydrochloride in solu- tion.     

Synthesis and Conformation of cis-1,2-Disubstituted Cyclododecene

Eight 1,2-disubstituted cyclododecenes were synthesized from a-alkoxycarbonyl-cyclododecanone and alkyl chloroformate. Their configuration and conformation determined by IR, NMR spectroscopy and X-ray diffraction analysis showed that the carbon-carbon double bond of all of the synthesized compounds has cis-configuration, and the ring skeleton of their preferred conformation is [lene2333] in solid, and they may adopt two different [lene2333] conformations, which exist in a dynamic equilibrium in solution.     

Operando HERFD-XANES and surface sensitive Δμ analyses identify the structural evolution of copper(Ⅱ) phthalocyanine for electroreduction of CO2

The quantitative understanding of how atomic-level catalyst structural changes affect the reactivity of the electrochemical CO₂reduction reaction is challenging.Due to the complexity of catalytic systems,conventional in situ X-ray spectroscopy plays a limited role in tracing the underlying dynamic structural changes in catalysts active sites.Herein,operando high-energy resolution fluorescence-detected X-ray absorption spectroscopy was used to precisely identify the dynamic structural transformation of well-defined active sites of a representative model copper(Ⅱ)phthalocyanine catalyst which is of guiding significance in studying single-atom catalysis system.Comprehensive X-ray spectroscopy analyses,including surface sensitive△μspectra which isolates the surface changes by subtracting the disturb of bulk base and X-ray absorption near-edge structure spectroscopy simulation,were used to discover that Cu species aggregated with increasing applied potential,which is responsible for the observed evolution of C₂H₄.The approach developed in this work,characterizing the active-site geometry and dynamic structural change,is a novel and powerful technique to elucidate complex catalytic mechanisms and is expected to con tribute to the rational design of highly effective catalysts.     

AN INVESTIGATION ON THE ab initio CALCULATION OF INTERMOLECULAR INTERACTION——NON-BONDED INTERACTION IN THE HYDROGEN BOND COMPLEX (HF)_2

An ab initio calculation of the hydrogen bond complex (HF)_2 is given with the 6-311 G~(**) basis set, according to which the potential surface around the balance point of the distancès and the orientations between two HF molecules is obtained. The atomic charges in the system are calculated with the PD/LSF method (potential-derived/least-square-fitting method) and then an analysis of the hydrogen bond interaction between two HF molecules is given with the (exp-6-1) potential function, by means of which it is shown that the main interaction between them is not an electro-static but a charge transfer one. The potential curve between two HF molecules is like a Morse function.     

Recent developments in two-dimensional (2D) correlation spectroscopy

Recent noteworthy developments in the field of two-dimensional(2D) correlation spectroscopy are reviewed.2D correlation spectroscopy has become a very popular tool due to its versatility and relative ease of use.The technique utilizes a spectroscopic or other analytical probe from a number of selections for a broad range of sample systems by employing different types of external perturbations to induce systematic variations in intensities of spectra.Such spectral intensity variations are then converted into2 D spectra by a form of correlation analysis for subsequent interpretation.Many different types of 2D correlation approaches have been proposed.In particular,2D hetero-correlation and multiple perturbation correlation analyses,including orthogonal sample design scheme,are discussed in this review.Additional references to other important developments in the field of 2D correlation spectroscopy,such as projection correlation and codistribution analysis,were also provided.     

Syntheses,Crystal Structures and Intermolecular Interactions of Cu（II） Complexes with Methyl- benzoic Acid （MBA） and 1,10-Phenanthroline

Two cupric complexes containing methylbenzoic acid have been prepared and crystallized by solvent evaporation method in DMF. The single-crystal X-ray crystallographic analysis reveals that they are dicaryon complexes. Complex I with formula of [Cu2（m- MBA）4DMF2] crystallizes in monoclinic with space group of P21/c and complex 2 with formula of [Cuz（o-MBA）ffo-phen）2]·NO3·H2O crystallizes in triclinic with space group of P I. The weak interactions including C-H...O hydrogen bonds, C-H…π interactions and π-π stacking in the structures of two complexes are observed from the X-ray crystallographic data. In addition, there are still classical hydrogen bonds in 2. The different strength of intermolecular interaction in the structure is reflected on their different thermal stability measured by thermal gravimetric analysis and 2D-1R correlation spectroscopy of two complexes. The study of weak interactions is meaningful to provide supporting data for supramolecular chemistry theory and potential applications in molecular biology.     

超声辅助法合成的石墨烯-TiO2复合材料声催化降解罗丹明B（英文）

A series of graphene-TiO2 composites was fabricated from graphene oxide and titanium n-butoxide(TNB) by an ultrasonic-assisted method.The structure and composition of the nanocomposites were characterized by Raman spectroscopy,BET surface area measurements,X-ray diffraction,transmission electron microscopy,and ultraviolet-visible absorption spectroscopy.The average size of the TiO2 nanoparticles on the graphene nanosheets was controlled at around 10-15 nm without using surfactant,which is attributed to the pyrolysis and condensation of dissolved TNB into TiO2 by ultrasonic irradiation.The catalytic activity of the composites under ultrasonic irradiation was determined using a rhodamine B(RhB) solution.The graphene-TiO2 composites possessed a high specific surface area,which increased the decolorization rate for RhB solution.This is because the graphene and TiO2 nanoparticles in the composites interact strongly,which enhances the photoelectric conversion of TiO2 by reducing the recombination of photogenerated electron-hole pairs.     

Syntheses,Crystal Structures and Photoluminescent Properties of Two New 1-D d~(10) Metal Complexes Based on Tetrazole 1-Acetato Ligand

Two new tetrazole 1-acetato complexes, [Ag(1-tza)(phen)]_∞(1) and [Cd(1-tza)2(2,2?-bipy)]∞(2)(1-Htza = tetrazole 1-acetato, phen = 1,10-phenanthroline, 2,2?-bipy = 2,2?-bipyridine), have been synthesized by solvothermal synthesis and structurally characterized by elemental analyses, IR spectra and single-crystal X-ray diffraction. Complex 1 shows a 1-D chained structure, while the structure of 2 contains two 1-D chains, which is the first 1-tza-based complex containing three different coordination modes of the 1-tza ligand. The aromatic stacking effects play an important role in the formation of supramolecular frameworks of these two complexes. Photoluminescent studies show that the two complexes exhibit efficient luminescence. In addition, optical diffuse reflectance spectra and thermogravimetric analyses of 1 and 2 have also been investigated.     

The Deactivation of Nickel Hydroxide to Hypophosphite Electrooxidation on a Nickel Electrode

The deactivation of nickel hydroxide to the electrooxidation of hypophosphite on a nickel electrode was studied by means of in situ UV-Vis subtractive reflectance spectroscopy. The experimental results show that when the potential is lower than -1.0 V (SCE), the surface on nickel electrode is free of nickel hydroxide, on which hypophosphite is active. When the potential moves positively to about 0.75V, two absorbency bands around 300nm and 550nm, which were ascribed to the formation of α-nickel hydroxide, were observed, nickel is oxidized to α-nickel hydroxide. Severe deactivation of the surface occurs when the nickel surface is covered with nickel hydroxide, which separates the hypophosphite ion from nickel substrate.     

Combination of Micro-fluidic Chip with Fluorescence Correlation Spectroscopy for Single Molecule Detection

A single molecule detection technique was developed by the combination of a single channel poly (dimethylsiloxane)/glass micro-fluidic chip and fluorescence correlation spectroscopy (FCS). This method was successfully used to determine the proportion of two model components in the mixture containing fluorescein and the rhodamine-green succinimidyl ester.     

An inverted triplesalen ligand by a convergent synthesis and its influence on trinuclear FeIII 3 complexes

The inverted triplesalen ligand H 6 feld Me has been synthesized from 2,4,6-triformyl-phloroglucinol and a ketimine salen half-unit in a convergent synthesis. NMR, IR, and UV-vis spectroscopy reveal that this ligand is not in the O-protonated tautomer but in the N-protonated tautomer with substantial heteroradialene contribution. This ligand and the conventional triplesalen ligand H 6 talen t-Bu 2 have been used to synthesize the trinuclear Fe III complexes [(feld Me )(FeCl) 3 ] and [(talen t-Bu 2 )(FeCl) 3 ], respectively. The molecular structures of these complexes were obtained by single-crystal X-ray diffraction. Two trinuclear Fe III complexes of [(feld Me )(FeCl) 3 ] dimerize via two Fe-phenolate bonds, whereas due to steric hindrance no dimerization is observed for [(talen t-Bu 2 )(FeCl) 3 ]. The structural data also reveal some heteroradialene contribution in the trinuclear complexes. Whereas UV-vis and M bauer spectroscopy are not suitable to distinguish between the two complexes, FT-IR spectra show characteristic features due to the different substitution patterns of the conventional and the inverted triplesalen ligands. Another handle is provided by electrochemistry. Whereas both complexes exhibit an irreversible oxidation wave (0.94 V vs. Fc + /Fc for [(feld Me )(FeCl) 3 ] and 0.84 V vs. Fc + /Fc for [(talen t-Bu 2 )(FeCl) 3 ]), which is assigned to the oxidation of the central backbone, higher potential oxidations are reversible for [(talen t-Bu 2 )(FeCl) 3 ]) but irreversible for [(feld Me )(FeCl) 3 ]. This is attributed to the reversible oxidation of the terminal phenolates in the di-tert-butyl substituted [(talen t-Bu 2 )(FeCl) 3 ] in contrast to the mono-methyl-substituted phenolates in [(feld Me )(FeCl) 3 ]. The magnetic properties of [(talen t-Bu 2 )(FeCl) 3 ] reveal a very small ferromagnetic coupling with significant zero-field splitting of the FeⅢ S = 5/2 ions. In contrast, the dimerization of two trinuclear complexes in [(feld Me )(FeCl) 3 ] results in antiferromagnetic interactions between the two phenolate-bridged Fe III ions, which mask the intra-trinuclear interactions transmitted by the central phloroglucinol backbone.     

Substituent effects on the EPR aN values of symmetrically para-disubstituted diphenyl nitroxides

Nitrogen hyperfine splitting constants (aN values) of seven symmetrically para-disubstituted diphenyl nitroxides (1-Y's) were measured by EPR and used in conjunction with five literature values in our correlation analysis. The correlation of these ON values by single-parameter Eq. 1 and dual-parameter Eq. 2 shows that the application of Eq. 2 does not significantly improve the correlation. But our data can also be interpreted by the proposition that the spin-delocalization effect is not completely nonexistent and that it might have revealed itself through the aN values of two very weakly polar substituents with pronounced spin-stabilizing abilities, i.e., SMe and SiMe3.     

STUDY OF XPS AND EHMO CALCULATION ON SILATRANE COMPOUNDS

Twenty silatrane compounds with different substituents(R) on the silicon atom are studied by means of X-ray photoelectron spectroscopy(XPS) and EHMO(extended Hückel molecular orbitals) theoretical calculation of the nine compounds in which substituents(R), F, Cl, Br, I, CH_3, H, CH=CH_2, CH_2Cl and CHCl_2, are carried out. By the X-ray photoelectron spectra of the component elements in these compounds, the existence of N→Si dative bond in these molecules is not only confirmed, but the affection of the different substituents on the strength of N→Si dative bond is also obtained. A linear correlation exists between atomic netcharge(Q) obtained by EHMO calculation and the binding energy shifts of N_1_g and Si_(2p) due to different substituents. The calculated bond orders can well predict the effect ou the strength of N→Si dative bond due to the change of substituents in the experiment. Meanwhile, the calculations indicate that the strength of N→Si dative bond in molecules of all substituents is about h     

Different J-Type Aggregates of meso-Tetrakis （4-hydroxyphenyl） porphyrin （H2THPP） Formed in Different Solvents

The aggregation of meso-tetrakis(4-hydroxyphenyl)porphyrin (H2THPP) in dimethylformamide (DMF)-water solution and in DMF-chloroform solution was studied by UV-vis absorption spectroscopy. The red shift of Soret band indicates the formation of J-type aggregates of H2THPP in these two solutions. However, different shift extent of Sorer band, 12 nm in DMF-water solution and 32 nm in DMF-chloroform solution, implies structural difference between these two J-type aggregates. The hydrogen bond between hydroxyl group and N-H bonds in porphyrin ring is thought as the main cause to the formation of J-type aggregate in DMF-chloroform solution, whereas the π-Q interaction between two adjacent porphyrin cores is thought as the main cause of the formation of J-type aggregate in DMF-water solution