Insights into the metabolite profiles of Rubus chingii Hu at different developmental stages of fruit

The fruits of Rubus chingii Hu have high medicinal and nutritional values. However, the metabolite profiles of R. chingii, especially the alterations during different development stages of fruit, have not been comprehensively analyzed, hindering the effective utilization of the unique species. In this study, we comprehensively analyzed the metabolites of R. chingii fruit at four developmental stages using systematic untargeted and targeted liquid chromatography-mass spectrometry metabolomics analysis and identified 682 metabolites. Significant changes were observed in metabolite accumulation and composition in fruits during the different developmental stages. The contents of the index components, kaempferol-3-O-rutinoside and ellagic acid, were the highest in immature fruit. The analysis identified 64 differentially expressed flavonoids and 39 differentially expressed phenolic acids; the accumulation of most of these differentially expressed metabolites decreased with the developmental stages of fruit from immaturity to maturity. These results confirmed that the developmental stages of fruit are a critical factor in determining its secondary metabolite compositions. This study elucidated the metabolic profile of R. chingii fruit at different stages of development to understand the dynamic changes in metabolites.     

Bacillus sphaericus asporogenous mutants: morphology,protein pattern and larvicidal activity

Asporogenous mutants from Bacillus sphaericus strains 2297 and 1593-4, blocked at different stages of the sporulation process, were isolated. Two mutants (2297 Aspo30A and 2297 Aspo34) which were blocked early in sporulation did not possess any crystalline inclusions and were poorly toxic to Culex pipiens mosquito larvae. Other mutants (2297 Aspo115, 2297 Aspo24 and 1593-4 Aspo12) which were blocked at later stages synthesized crystal-like inclusions next to the forespores, and were highly toxic to mosquito larvae. Electrophoretic protein analysis of alkali extracts from mutants and wild type strains confirmed the absence of toxic crystal-related proteins in early-blocked mutants and their presence in later ones. Western blots with antisera directed against the crystal proteins confirmed those observations.     

Use of the photoluminescence intensity variation as an in-situ probe for electrochemical copper deposition on a p-type GaAs electrode

Photoluminescence was used as an in-situ method for following the electrodeposition of copper on p-type GaAs electrodes from a 0.5 M H₂SO₄ solution containing Cu(II) sulphate. The method appeared to be very sensitive to copper coating and to be able to detect a copper amount of the monolayer range. Moreover, during anodic polarisation of the metallised electrode, photoluminescence measurements showed the complete dissolution of the copper layer. In-situ photoluminescence measurements were confirmed by ex-situ analyses at different stages of the electrochemical treatment of the GaAs electrode.     

Study of thermal behavior of α-PbO2, using TG and DSC

Using two techniques of thermogravimetry and differential scanning calorimetry under O₂ gas atmosphere from 25 to 600°C, the thermal behavior of laboratory-produced compound lead(IV) oxide α-PbO₂ was investigated. The identity of products at different stages were confirmed by XRD technique. Both techniques produced similar results supporting the same decomposition stages for the compound. Three distinct energy changes were observed, namely, two endothermic and one exothermic in DSC. The amount of ΔH for each peak is also reported.     

Inhibitory effect of the mixtures of phenol antioxidants and phosphatidylcholine

Phospholipids, phosphatidylcholine from egg yolk (PC) and dipalmitoylphosphatidylcholine, in a complex way affect the inhibitory action of phenol antioxidants (InH) during initiated oxidation of ethylbenzene. At the initial stages of the reaction, phospholipids decrease the efficiency of inhibition by InH. This effect was described satisfactorily with a kinetic scheme that includes the formation of the complex InH · PC, which is inactive in inhibition. The formation of this complex was confirmed spectrophotometrically. Prolongation of the inhibitory effect of the mixture of PC with 4-methoxyphenol compared to the effect of InH alone was found. The effect of PC on the efficiency of inhibition by InH also depends on the duration of the oxidation reaction.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1053–1059, June, 1995.     

Synthetic TRPO<Subscript>4</Subscript> crystals as reference samples in the quantitative X-ray electron probe microanalysis of rare-earth elements

Crystals of 15 rare-earth element phosphates, which provide a set of standard reference samples in X-ray electron probe microanalysis, were synthesized and tested for homogeneity and stoichiometry. The phosphates were synthesized in two stages, the preparation of aqueous phosphates and crystal growth in a solution of potassium polymolybdate K₂Mo₃O₁₀. The tests of the synthesized crystals confirmed their reliability as reference samples.     

Thermal analysis of mechanoactivated mixtures of tunisia phosphorite and ammonium sulfate

The thermal behavior of Tunisia phosphorite and ammonium sulfate mixtures are examined by non-isothermal thermogravimetry in air atmosphere. It has been shown that the thermal stability of mixtures have different behavior after mechano-chemical treatment due to phase changes in the mixtures. New solid phases are confirmed by the stages and rate of mass changes and also by the heat effects observed. New phases are also confirmed by using X-ray diffraction method. Based on the data obtained by the mechanism of chemical transformations is proposed. The kinetics of mechano-activated mixtures decomposition is significantly influenced by the time of treatment and proceeds in few stages. Stage I is attributed to the effect of partially ammonia releasing, when the next stages are associated with the decomposition of apatite structures. Because of the interfacial interactions during mechano-chemical treatment insoluble phosphorous forms from apatite structures are transformed to the soluble forms suitable for plants nutrition. The results have shown that the soluble form can be controlled by the initial components ratio and conditions of treatment on the way to obtain slow releasing nutrition products. This revised version was published online in July 2006 with corrections to the Cover Date.     

DSC and adiabatic calorimetry study of the polymorphs of paracetamol

Monoclinic (I) and orthorhombic (II) polymorphs of paracetamol were studied by DSC and adiabatic calorimetry in the temperature range 5 - 450 K. At all the stages of the study, the samples (single crystals and powders) were characterized using X-ray diffraction. A single crystal → polycrystal II→ I transformation was observed on heating polymorph II, after which polymorph I melted at 442 K. The previously reported fact that the two polymorphs melt at different temperatures could not be confirmed. The temperature of the II→I transformation varied from crystal to crystal. On cooling the crystals of paracetamol II from ambient temperature to 5 K, a II→ I transformation was also observed, if the 'cooling-heating' cycles were repeated several times. Inclusions of solvent (water) into the starting crystals were shown to be important for this transformation. The values of the low-temperature heat-capacity of the I and II polymorphs of paracetamol were compared, and the thermodynamic functions calculated for the two polymorphs. This revised version was published online in July 2006 with corrections to the Cover Date.     

Dynamics of structural transformations in the reduction of copper aluminate

The dynamics of structural transformations during copper aluminate reduction in the temperature range used for catalyst activation was studied by high-temperature X-ray analysis under controlled conditions (hydrogen, 2O–4OO‡C). The techniques of neutron diffraction analysis, IR spectroscopy, chemical phase analysis, and electron microscopy were also used at particular stages. In the course of reduction, copper metal is deposited onto the surface of spinel crystals from the bulk. Spinel becomes cation-deficient with respect to copper. An analysis of powder diffraction patterns demonstrated that copper is reduced and released from tetrahedral positions of the spinel structure at temperatures below ~300‡C and from octahedral positions only at temperatures above 300‡C. In this case, a redistribution of aluminum ions was observed simultaneously. It is likely that the electrical neutrality is attained by the formation of OH groups, the appearance of which in reduced samples was detected by IR spectroscopy and confirmed by neutron diffraction analysis. At a reduction temperature of 400‡C, the oxygen framework was partially disintegrated. The structures of reduced copper aluminates and chromites were compared.     

Preparation of high-purity thorium by solvent extraction with di-(2-ethylhexyl) 2-ethylhexyl phosphonate

The extraction behavior of thorium(IV) by di-(2-ethylhexyl) 2-ethylhexyl phosphonate (DEHEHP, B) from nitric acid media has been investigated. The influence factors including the concentration of HNO₃, salting-out reagents, temperature, the concentration of metal ions and DEHEHP have been examined systematically. A possible extraction mechanism is proposed and the extracted species as Th(NO₃)₄·2B _(o) is confirmed by the slope analysis method. The extraction equilibrium constants (K _ex) and thermodynamic parameters (ΔG, ΔH and ΔS) were calculated under the present experimental conditions. DEHEHP shows a high selectivity of thorium(IV) over rare earths(III). Stripping study indicates that thorium can be completely stripped by distilled water from the Th-loaded DEHEHP. Furthermore, a solvent extraction process including six extraction stages, six scrubbing stages, and six stripping stages was designed for the preparation of highly pure thorium from thorium concentrate with DEHEHP as extractant in laboratory scale, and finally thorium product can be obtained with a purity of 99.999 % and a yield of 98 %.     

Analysis of the release process of phenylpropanolamine hydrochloride from ethylcellulose matrix granules II. effects of the binder solution on the release process

The release properties of phenylpropanolamine hydrochloride (PPA) from ethylcellulose (EC) matrix granules prepared by an extrusion granulation method were examined. The release process could be divided into two parts; the first and second stages were analyzed by applying square-root time law and cube-root law equations, respectively. The validity of the treatments was confirmed by the fitness of a simulation curve with the measured curve. In the first stage, PPA was released from the gel layer of swollen EC in the matrix granules. In the second stage, the drug existing below the gel layer dissolved and was released through the gel layer. The effect of the binder solution on the release from EC matrix granules was also examined. The binder solutions were prepared from various EC and ethanol (EtOH) concentrations. The media changed from a good solvent to a poor solvent with decreasing EtOH concentration. The matrix structure changed from loose to compact with increasing EC concentration. The preferable EtOH concentration region was observed when the release process was easily predictable. The time and release ratio at the connection point of the simulation curves were also examined to determine the validity of the analysis.     

Formation and structure of anisotropic gels III.: Electron-microscopic investigation of the formation process of calcium alginate laminated gels

Summary Formation of calcium alginate laminated gels proceeds at least in two stages: at first a reticular structure is formed that then transforms into a compact structure, the transition rate decreasing with the increase of alginate concentration. The fibrillar nature of the reticular structure is confirmed by freeze-drying studies.With 4 figures     

多层螺旋CT多平面重建在胃肠道淋巴瘤诊断中的应用及与临床分期的相关性研究

为研究多层螺旋CT多平面重建在胃肠道淋巴瘤诊断中的应用价值及检测结果与临床分期的相关性,本次研究筛选我院2016年1月~2019年6月收治的50例经病理学检查证实的胃肠道淋巴瘤患者为观察组,另选同期50例非胃肠道淋巴瘤患者为对照组,均实施多层螺旋CT多平面重建,对比两组及观察组内不同组织类型、不同临床分期患者CT重建参数(图像客观噪声、信噪比)的差异,利用Pearson相关性分析法对CT重建参数与胃肠道淋巴瘤临床分期的相关性进行检验。病理学检查证实,50例胃肠道淋巴瘤患者中有弥漫性大B细胞淋巴瘤25例、黏膜相关淋巴瘤19例、小B细胞淋巴瘤4例、套细胞淋巴瘤2例,与多层螺旋CT多平面重建符合率差异无统计学意义(P>0.05)。观察组图像客观噪声低于对照组,信噪比高于对照组,差异有统计学意义(P<0.05)。观察组内不同组织类型患者、不同临床分期患者CT重建参数差异有统计学意义(P<0.05)。Pearson相关性分析结果提示,多层螺旋CT多平面重建参数中图像客观噪声与胃肠道淋巴瘤临床分期呈负向相关性(r=-0.74,P<0.05),信噪比与胃肠道淋巴瘤临床分期呈正相关性(r=0.71,P<0.05)。据此可得,在胃肠道淋巴瘤诊断中多层螺旋CT多平面重建取得的效果更佳且CT重建参数与临床分期密切相关,对于辨别组织类型和判断临床分期具有重要参照价值,值得推广。     

Interactions during the chlorination of a copper–zinc alloy

In this paper several aspects involved in the chlorination of a Zn 48% wt.–Cu alloy between 250 and 500 °C are investigated. The starting temperature for the chlorination of the alloy is determined, which is different from those of pure metals. Analysis of the chlorination thermogravimetric curves and reaction products reveal that there are interactions between reactants and products during the reaction, and that volatilization of ZnCl₂ is diminished during the alloy chlorination. Metallic copper is detected at intermediate stages of the chlorination, and this element, which is not present in the initial sample, appears during the chlorination reaction. An oxidation–reduction type reaction between copper chlorides and metallic zinc is proposed to explain the behaviour observed. The occurrence of this reaction at room temperature was confirmed in separate experiments. At the beginning of the reaction, formation of zinc oxichloride was detected that is being formed from the zinc oxide layer that covers the alloy surface. According to the results obtained, a reaction mechanism is presented for the alloy chlorination.     

Fundamental study on the thermal regeneration stages of exhausted activated carbons: kinetics

In this work the thermal regeneration of activated carbons saturated with p-nitrophenol has been analysed. By thermogravimetry, it was possible to elucidate the different events taking place during the thermal treatment, and relate them to the type of adsorption in the interfacial system. It was found that the mass loss during thermal treatment comprises a complex process in which different stages are involved, such as drying, desorption of physisorbed adsorbate, breaking up of surface functional groups, cracking of products from adsorbate–surface-specific interactions, etc. The analysis of the textural and surface chemistry characteristics of the pristine and regenerated adsorbent confirmed the thermal desorption mechanisms. Moreover, a kinetic study based on temperature-programmed desorption and Suzuki models was performed, using thermogravimetry data at different heating rates (5–20 K min^?1). From this analysis, the values of activation energy involved in each degradation step were estimated.     

n-Alkanoic acid monolayers on 316L stainless steel promote the adhesion of electropolymerized polypyrrole films

The formation of a self-assembled monolayer significantly promotes the adhesion of electrodeposited polypyrrole on stainless steel. The monolayer affects the nucleation and growth mechanism of polypyrrole as a result of its hydrophobic nature. This was confirmed by analyzing current-time transients of the initial stages of electropolymerization and was in agreement with AFM images.     

Natural phenolic compounds in the reaction with a nitrogen-centered radical in an aprotic solvent

Kinetics and mechanism of the reaction of vegetable phenols (PhOH) with 2,2′-diphenyl-1-picrylhydrazyl radical (DPPH?) in a polar aprotic solvent, dimethyl sulfoxide, were studied. The reaction of natural phenols with DPPH? in dimethyl sulfoxide occurs in two stages. In the first stage, a proton-coupled electron transfer (PCET) occurs from a PhOH molecule to DPPH? to give primary transformation products, phenoxyl radicals (PhO?) and diphenyl hydrazine (DPPH–H), and in the second, the hydrazyl radical is consumed in the reaction with PhO? transformation products, enolized dimers, which is confirmed by NMR spectroscopy. A relationship was revealed between the antiradical activity of phenols in the reaction with DPPH? (ln k) and the ionization potential of the phenolates being formed.     

Evaluation of Structure,Nucleation and Growth Mechanism of Electropolymerized Polypyrrole on Highly Oriented Pyrolytic Graphite Electrode

Chronoamperometry (i–t) and atomic force microscopy (AFM) were used to study the nucleation and growth mechanism of electropolymerized polypyrrole formed on highly oriented pyrolytic graphite (HOPG) substrate surface. From i–t measurements it was found that the nucleation and growth mechanism was a 3‐D progressive after nuclei overlapping. However, before nuclei overlapping, it was not clear whether the mechanism was 2‐D instantaneous or 3‐D progressive. This ambiguity in the nucleation and growth mechanism was confirmed as 3‐D progressive from the results of AFM measurements. In addition to nucleation and growth mechanism, possible models were proposed for different structures observed on the AFM image of polypyrrole, obtained from very early stages of polymerization.     

A novel sulfur containing C35 hopanoid in sediments.

A C₃₅ pentacyclic triterpenoid of the hopane series containing a thiophene ring, 30-(2′-methylene thienyl)-17β(H),21β(H)-hopane 1, has been confirmed in immature sediments by synthesis, suggesting incorporation of bacterial sulfur into geological organic matter at early stages of sedimentation.     

The impact of the concentration of casein micelles and whey protein-stabilized fat globules on the rennet-induced gelation of milk

The rennet-induced aggregation of skim milk recombined with whey protein-stabilized emulsion droplets was studied using diffusing wave spectroscopy (DSW) and small deformation rheology. The effect of different volume fractions of casein micelles and fat globules was investigated by observing changes in turbidity (1/l*), apparent radius, elastic modulus and mean square displacement (MSD), in addition to confocal imaging of the gels.Skim milk containing different concentration of casein micelles showed comparable light-scattering profiles; a higher volume fraction of caseins led to the development of more elastic gels.By following the development of 1/l* in recombined milks, it was possible to describe the behaviour of the fat globules during the initial stages of rennet coagulation. Increasing the volume fraction of fat globules showed a significant increase in gel elasticity, caused by flocculation of the oil droplets. The presence of flocculated oil globules within the gel structure was confirmed by confocal microscopy observations. Moreover, a lower degree of κ-casein hydrolysis was needed to initiate casein micelles aggregation in milk containing whey protein-stabilized oil droplets compared to skim milk.This study for the first time clearly describes the impact of a mixture of casein micelles and whey protein-stabilized fat globules on the pre-gelation stages of rennet coagulation, and further highlights the importance of the flocculation state of the emulsion droplets in affecting the structure formation of the gel.