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Objective. X-ray diffraction (XRD) technology uses x-ray small-angle scattering signal for material analysis, which is highly sensitive to material inter-molecular structure. To meet the high spatial resolution requirement in applications such as medical imaging, XRD computed tomography (XRDCT) has been proposed to provide XRD intensity with improved spatial resolution from point-wise XRD scan. In XRDCT, 2D spatial tomography corresponds to a 3D reconstruction problem with the third dimension being the XRD spectrum dimension, i.e. the momentum transfer dimension. Current works in the field have studied reconstruction methods for either angular-dispersive XRDCT or energy-dispersive XRDCT for small samples. The approximations used are only suitable for regions near the XRDCT iso-center. A new XRDCT reconstruction method is needed for more general imaging applications. Approach. We derive a new FDK-type reconstruction method (Reciprocal-FDK) for XRDCT without limitation on object size. By introducing a set of reciprocal variables, the XRDCT model is transformed into a classical cone-parallel CT model, which is an extension of a circular-trajectory cone-beam CT model, after which the FDK method is applied for XRDCT reconstruction. Main results. Both analytical simulation and Monte Carlo simulation experiments are conducted to validate the XRDCT reconstruction method. The results show that when compared to existing analytical reconstruction methods, there are improvements in the proposed Reciprocal-FDK method with regard to relative structure reconstruction and XRD pattern peak reconstruction. Since cone-parallel CT does not satisfy the data completeness condition, cone-angle effect affects the reconstruction accuracy of XRDCT. The property of cone-angle effect in XRDCT is also analyzed with ablation studies. Significance. We propose a general analytical reconstruction method for XRDCT without constraint on object size. Reciprocal-FDK provides a complete derivation and theoretical support for XRDCT reconstruction by analogy to the well-studied cone-parallel CT model. In addition, the intrinsic problem with the XRDCT data model and the corresponding reconstruction error are discussed for the first time.

Drug combinations have been the hotspot of the pharmaceutical industry, but the promising applications are limited by the unmet solubility and low bioavailability. In this work, novel cocrystals, consisting of two antithrombotic drugs with poor solubility and low bioavailability in vivo, namely, apixaban (Apx) and quercetin (Que), were developed to discover a potential method to improve the poor solubility and internal absorption of the drug combination. Compared with Apx, the dissolution behavior of Apx–Que (1:1) and Apx–Que–2ACN (1:1:2) was enhanced significantly, while the physical mixture of the chemicals failed to exhibit the advantages. The dissolution improvements of Apx–Que–2ACN could be explained by the fact that the solid dispersion-like structure and column-shaped cage of Que accelerated the access of the solvent to the inner layer of Apx. The fracture of the hydrogen bonds of Apx, which was the joint of the adjacent Que chains, facilitated the break-up of the structures. Besides, the bioavailability of Apx–Que was increased compared with the physical mixture and Apx, and Apx–Que remained stable in high temperature and illumination conditions. Therefore, a drug–drug cocrystal of two antithrombotic agents with poor solubility was developed, which exhibited greatly improved solubility, bioavailability and superior stability, indicating a novel method to overcome the shortages of drug combination.

In order to improve the mechanical properties of nano hydroxyapatite (HA), silicon carbide whisker (SiCw) with excellent mechanical and biological properties was used as the reinforcement for SiC whisker reinforced nano hydroxyapatite (SiCw/HA) composites. Hydrothermal synthesis method was adopted to prepare the uniformly dispersed SiCw and HA composite powders, and SiCw/HA composites were fabricated by pressureless sintering. The interfacial bonding state and mechanical properties of SiCw/HA composites in different sintering atmospheres (air and N2) were systematically investigated. The results show that the uniformity of the composite powders decreases with the increase of SiCw content, and the cross-section of SiCw/HA composites gradually changes from glossy and smooth to rough and undulate. When the content of SiCw is 15 wt%, the maximum bending strength and fracture toughness of the composites sintered in air atmosphere (HAW15) are 40.85 MPa and 1.82 MPa·m1/2 respectively, which are higher than those of pure HA. Compared with those of the SiCw/HA composites sintered in N2 atmosphere, the bending strength and fracture toughness of the HAW15 composites are increased by 154.2% and 10.3%, respectively. Moreover, Simulated body fluid (SBF) and in vitro cell behavior tests indicate that the SiCw/HA composites still have excellent bioactivity. The possible strengthening and toughening mechanisms of SiCw/HA composites are that the dispersion of SiCw in HA matrix is improved by hydrothermal process, and the interfacial bonding property is enhanced because of the reaction fusion on interface of SiCw/HA composites during sintering in air atmosphere. The adoption of hydrothermal process improves the dispersion uniformity of SiCw in HA matrix. When sintering in air atmosphere, the interfacial bonding property of SiCw/HA composite is enhanced via the reaction fusion (SiO2 is formed by the oxidation of SiCw). Both of them lead to the increase of strength and toughness of the composites. This study would provide additional insights into the feasibility of SiCw/HA composites as load-bearing implant materials in orthopedic applications.

An ionic liquid of N-methylmorpholine-N-oxide (NMMO) was used to effectively pretreat cassava residues for the efficient enzymatical hydrolysis and cogeneration of fermentative hydrogen and methane. The reducing sugar yield of enzymolysed cassava residues with NMMO pretreatment improved from 36 to 42g/100g cassava residues. Scanning electron microscopy images revealed the formation of deep grooves (∼4μm wide) and numerous pores in the cassava residues pretreated with NMMO. X-ray diffraction patterns showed that the crystallinity coefficient of NMMO-pretreated cassava residues decreased from 40 to 34. Fourier transform infrared spectra indicated that crystal cellulose I was partially transformed to amorphous cellulose II in the NMMO-pretreated cassava residues. This transformation resulted in a reduced crystallinity index from 0.85 to 0.77. Hydrogen yield from the enzymolysed cassava residues pretreated with NMMO increased from 92.3 to 126mL/gTVS, and the sequential methane yield correspondingly increased from 79.4 to 101.6mL/g TVS.

Four new solvatomorphs of betulin were reported and characterized by X-ray diffractometry as well as thermal and vibrational spectroscopic analyses. Single-crystal X-ray diffraction was used to analyze the X-ray structures of the compounds and confirmed the stoichiometric ratio between the host and guest molecules from thermal data. Results indicated that solvatomorphism occurred in several betulin solvates. Changes in intermolecular arrangements, stoichiometry, and hydrogen-bonding interactions of solvatomorphs were due to solvent incorporation to solvates. Hirshfeld surface analyses, especially d norm surface and fingerprint plots, were used to determine intermolecular interactions in the crystal network. Solvent molecules played an important role in the construction of a 3D architecture. The stabilities of these solvates were evaluated by thermal analyses. Nonisothermal kinetic analysis was used to explain the kinetics of solid–solid phase transition (desolvation) of betulin solvates. The apparent activation energies were evaluated using Kissinger and Ozawa methods. Moreover, phase transitions were visually investigated by hot-stage microscopic analysis.

Non-enzymatic glucose sensors are attracting significant attention owing to their low cost, storage convenience and reusability; however, their poor anti-interference caused by their weak selectivity towards glucose limits their practicability. In the present study, a MIL-53(NiFe) metal-organic framework (MOF) was prepared on Ni foam to serve as a self-supported electrode for non-enzymatic glucose detection. Due to the abundant active sites in the MIL-53(NiFe) MOF and its good stability in an alkaline solution, the sensors exhibited a high sensitivity (41.95 mA mM-1 cm-2) and a low detection limit (0.67 μM). Moreover, the molecular sieve effect of the MIL-53(NiFe) MOF led to a remarkable anti-interference ability, even at the interference concentrations of up to 20% glucose, a higher value than that in human serum. In addition, a heat treatment was carried out to remove the residual terephthalic acid in the MOF tunnels, and this promoted the detection linear range to 2-1600 μM. The reusability, reproducibility and long-term stability of the sensors were also studied, and the results implied good practicability of the MIL-53(NiFe) MOF-based sensors. Furthermore, the good practicability of the sensors was verified by testing human serum samples. The results showed the relative standard deviation of 2.73% from the hospital results, and the standard recovery was nearly 100%.

Molecular imaging is of significant importance for early detection and diagnosis of cancer. Herein, a novel core-shell magnetic microsphere for dual modal magnetic resonance imaging (MRI) and optical imaging was produced by one-pot emulsifier-free emulsion polymerization, which could provide high resolution rate of histologic structure information and realize high sensitive detection at the same time. The synthesized magnetic microspheres composed of cores containing oleic acid (OA) and sodium undecylenate (NaUA) modified Fe3O4 nanoparticles and styrene (St), Glycidyl methacrylate (GMA), and polymerizable lanthanide complexes (Gd(AA)3Phen and Eu(AA)3Phen) polymerized on the surface for outer shells. Fluorescence spectra show characteristic emission peaks from Eu(3+) at 590nm and 615nm and vivid red fluorescence luminescence can be observed by 2-photon confocal scanning laser microscopy (CLSM). In vitro cytotoxicity tests based on the MTT assay demonstrate good cytocompatibility, the composites have longitudinal relaxivity value (r1) of 8.39mM(-1)s(-1) and also have transverse relaxivity value (r2) of 71.18mM(-1)s(-1) at clinical 3.0 T MR scanner. In vitro and in vivo MRI studies exhibit high signal enhancement on both T1- and T2-weighted MR images. These fascinating multifunctional properties suggest that the polymer microspheres have large clinical potential as multi-modal MRI/optical probes.

Synthesized organobentonite (SOB), montmorillonite (MMT), and commercial organobentonite (COB) were used as adsorbents for paraffin oil, a model pollutant in land-based oil spills and oil pipeline rupture. The characterization of clays was carried out with scanning electron microscopy (SEM), thermogravimetric analysis (TG), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). After adsorption, oil was separated from adsorbents with a carbon dioxide responsive solvent N,N-dimethylcyclohexylamine (DMCHA), and DMCHA was subsequently separated from paraffin oil upon CO2 bubbling instead of distillation with high energy cost. The adsorption capacity of oil to SOB, MMT, and COB was 0.686, 1.124, and 1.239 g/g, respectively. It was found that the adsorption capacity and rinsed amount of the adsorbents depended on the d-spacing, which is related to surfactant content. Electrical conductivity and pH measurements suggested that the separation process occurred via two steps. Firstly, during the initial 35 min, carbonate ions coexisted with bicarbonate ions. Then, only bicarbonate ions existed after the introduction of CO2 gas for 120 min. Thus, organobentonites were feasible for hydrocarbon adsorption and could be simply reused by an amine-based responsive solvent. This work provided a cost-effective and sustainable method of recycling of organobentonites and the responsive solvent, which can be used to deal with leaked oil and oil spills.

To improve the photocatalytic efficiency of chromium-based metal-organic framework (MIL-101) photocatalyst, Pd nanoparticles and reduced graphene oxide were used to modify the MIL-101 via a facile method. The resulting novel photocatalyst was characterized by UV-vis diffuse reflectance spectra (DRS), powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). It was indicated that the photocatalyst afforded high photocatalytic efficiency for degradation of two triphenylmethane dyes, brilliant green and acid fuchsin, under exposure to visible light irradiation. Cyclic experiments demonstrated that the photocatalyst showed good reusability and stability for the dye degradation.

The Bam machinery, which is highly conserved from bacteria to humans, is well recognized as the apparatus responsible for the insertion and folding of most outer membrane proteins in Gram-negative bacteria. InEscherichia coli, the Bam machinery consists of five components (i.e.BamA, BamB, BamC, BamD and BamE). In comparison, there are only four partners inHaemophilus influenzae: a BamB homologue is not found in its genome. In this study, the recombinant expression, purification, crystallization and preliminary X-ray diffraction analysis ofH. influenzaeBamD and BamCD complex are reported. The genes encoding BamC and BamD were cloned into a pET vector and expressed inE. coli. Affinity, ion-exchange and gel-filtration chromatography were used to obtain high-purity protein for further crystallographic characterization. Using the hanging-drop vapour-diffusion technique, BamD and BamCD protein crystals of suitable size were obtained using protein concentrations of 70 and 50 mg ml−1, respectively. Preliminary X-ray diffraction analysis showed that the BamD crystals diffracted to 4.0 Å resolution and belonged to space groupP212121, with unit-cell parametersa= 54.5,b= 130.5,c= 154.7 Å. The BamCD crystals diffracted to 3.8 Å resolution and belonged to space groupI212121, with unit-cell parametersa= 101.6,b= 114.1,c= 234.9 Å.

Purpose: Improving the peri-implant bone quality has notable clinical value in cases of osteoporosis following implant insertion. Materials and Methods: In this study, strontium ranelate–loaded chitosan film was produced on a titanium surface in different concentrations of strontium ranelate (SR) (0, 2, 20, 40, and 80 mmol/L of the strontium ion [Sr2+]) with the expectation of utilizing the bone healing–enhancement effect of Sr2+. The physicochemical properties of SR-loaded chitosan films were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The release/dissolution mechanism was tested by inductively coupled plasma optical emission spectrometry (ICP-OES), and in vitro cell responses were evaluated using primary osteoblasts (POBs) in terms of cell proliferation, alkaline phosphatase (ALP) activity, and quantitative analysis of key osteoblastic gene expression. Results: XRD and FTIR observation showed that only a few SRs reacted chemically with chitosan through hydrogen bonds or conjugate action. The initial burst release (70% to 85%) of Sr2+ occurred in the first 3 days and was followed by a slower release stage. At a low concentration (2 mmol/L or 20 mmol/L), SR-loaded chitosan film promoted cell responses of POBs with enhanced proliferation, ALP activity, and expression levels of bone morphogenetic protein 2 (BMP-2), runt-related transcription factor 2 (Runx-2), ALP, and osteocalcin, but at a high concentration (40 mmol/L or 80 mmol/L), it inhibited POB growth. Conclusion: These results indicated that SR-loaded chitosan film on a titanium surface promotes osteoblast proliferation and differentiation in a dose-dependent manner, which may represent a new approach in the treatment of a titanium implant.

Recent advances in experimental techniques and data processing allow in situ determination of mineral crystal structure and chemistry up to Mbar pressures in a laser-heated diamond anvil cell (DAC), providing the fundamental information of the mineralogical constitution of our Earth's interior. This work highlights several recent breakthroughs in the field of high-pressure mineral crystallography, including the stability of bridgmanite, the single-crystal structure studies of post-perovskite and H-phase as well as the identification of hydrous minerals and iron oxides in the deep lower mantle. The future development of high-pressure crystallography is also discussed.

A large number of rare earth element mining and application resulted in a series of problems of soil and water pollution. Environmental remediation of these REE-contaminated sites has become a top priority. This paper explores the use of Bacillus licheniformis to adsorb lanthanum and subsequent mineralization process in contaminated water. The maximum adsorption capacity of lanthanum on bacteria was 113.98 mg/g (dry weight) biomass. X-ray diffraction (XRD) and transmission electron microscopy (TEM) data indicated that adsorbed lanthanum on bacterial cell surface occurred in an amorphous form at the initial stage. Scanning electron microscopy with X-ray energy-dispersive spectroscopy (SEM/EDS) results indicated that lanthanum adsorption was correlated with phosphate. The amorphous material was converted into scorpion-like monazite (LaPO4 nanoparticles) in a month. The above results provide a method of using bacterial surface as adsorption and nucleation sites to treat REE-contaminated water.

Synchrotron radiation (SR) based techniques have been utilized with increasing frequency in the past decade to explore the brilliant and challenging sciences of actinide-based materials. This trend is partially driven by the basic needs for multi-scale actinide speciation and bonding information and also the realistic needs for nuclear energy research. In this review, recent research progresses on actinide related materials by means of various SR techniques were selectively highlighted and summarized, with the emphasis on X-ray absorption spectroscopy, X-ray diffraction and scattering spectroscopy, which are powerful tools to characterize actinide materials. In addition, advanced SR techniques for exploring future advanced nuclear fuel cycles dealing with actinides are illustrated as well.

During photodynamic therapy (PDT) of cancers, there are numerous side effects, accompanied by damage to normal cells/tissues caused by the abnormal elevation of reactive oxygen species (ROS). In this paper, we aim to provide an effective method to reduce the relevant side effects of PDT by using cerium oxide nanoparticles. The well-dispersed poly(vinyl pyrrolidone) stabilized cerium oxide nanoparticles were successfully synthesized by using a one-pot method at 60 degrees C in slightly alkaline environment. The morphological and structural characterizations clearly illustrate the excellent lattice structures of cerium oxide, nanoparticles. The MTT assay indicates that these cerium oxide nanoparticles show no intrinsic cytotoxicity even at a concentration up to 300 micro g/mL. More importantly, the results demonstrate that these nanoparticles can selectively protect human normal cells but not the cancer cells from ROS damage after exposure to UV-radiation, suggesting their potential applications for PDT treatment. The rationale behind the selective protection effect can be attributed to the hindrance of the Ce (III)/Ce (IV) redox reaction cycle on the surface of cerium oxide nanoparticles due to the abnormal intracellular pH in cancer cells. Furthermore, these cerium oxide nanoparticles can be used as effective drug carriers for enhancing drug delivery efficiency to target cancer cells like hepatoma HepG2 cells. This raises the possibility of applying cerium oxide nanoparticles for multifunctional therapeutic applications, i.e., combination of efficient PDT and chemotherapy.

Purpose This study compared the effect of magnesium-incorporated hydroxyapatite (MgHA) coating with that of HA coating on implant fixation in ovariectomized (OVX) rats. Materials and methods Coatings of HA and MgHA (10 mol% Ca²⁺ replaced by Mg²⁺) were prepared on the surface of titanium substrates using the sol-gel dip-coating method, and powders of HA and MgHA were produced by the same method. The two kinds of materials were then characterized by scanning electron microscopy and x-ray diffraction. Twelve weeks after bilateral ovariectomy, 18 OVX rats received implants in the distal femora; half of the implants were HA-coated and the other half were MgHA-coated. After 12 weeks of healing, rats were selected randomly for histomorphometry, microcomputed tomography evaluation, and biomechanical testing. Results Surface characterization analysis demonstrated that the addition of Mg did not dramatically change the surface topography or apatite patterns of the coating. Histomorphometry revealed higher bone-to-implant contact and bone area ratio for MgHA-coated implants than for HA-coated implants. Microcomputed tomographic evaluation revealed improved trabecular parameters and increased osseointegration for MgHA-coated implants. Biomechanical testing revealed that the MgHA coating increased the maximum push-out force and interfacial shear strength compared to the HA coating. Conclusion Mg incorporated into an HA coating on titanium implants could improve the biologic fixation of implants in osteoporotic bone.

The cosine-model analysis (CMA) method and the small angle x-ray scattering (SAXS) method are two major types of information retrieval algorithms, commonly utilized in x-ray phase-contrast imaging with a grating interferometer. However, there are significant differences between the two methods in algorithm implementation, and the existing literature has not completely revealed their intrinsic relationship. In this paper, we theoretically derive and experimentally verify the intrinsic connections between CMA and SAXS, and it is seen that SAXS can be interpreted well by the cosine-model assumption of CMA. To validate our analysis of the scattering distribution when applying the cosine model to the convolution used in SAXS, we applied a deconvolution process into CMA before using the Fourier transform to get the three contrasts. Furthermore, the principal component analysis (PCA) is introduced in this work, and two PCA-based retrieval algorithms are presented in order to simplify the iteration process of deconvolution in SAXS or to obtain absorption and dark-field signals instead of the Fourier transform in CMA. Applying a quantitative structural similarity (SSIM) index and a profile analysis to the results of an ex vivo mammography, it is proved that retrieved images via CMA and SAXS are consistent with each other (SSIM values are 1.0000, 0.9845 and 0.9767 respectively), and that the extra deconvolution process applied into CMA shows a good performance and our analytical analysis of the scattering distribution is valid when applying the cosine model to the convolution used in SAXS. Besides, it is concluded that PCA shows almost the same performance with the Fourier transform (SSIM values are 1.0000 for both absorption and dark-field images), and the simplified SAXS-analogous method works well with higher efficiency in computation and better stability relative to the original SAXS, while maintaining the similar level of image quality (SSIM values are 1.0000, 0.9839 and 0.9781 respectively).

Our purpose is to describe the characteristics and the outcome of melamine-induced renal and urinary tract injury in young children who consumed melamine-contaminated infant formula.This is a descriptive longitudinal study over 2 years in 240 children with melamine-induced urolithiasis screened in our hospital from September 15 to October 31, 2008. Ultrasonography and serum creatinine (SCr), urea, β2-microglobulin (MG), cystatin C (Cys C), urinary Cr (UCr), microalbumin (mALB), α1-MG, β2-MG, n-acetyl-β-d-glucosaminidase (NAG) and retinol-binding protein (RBP) measurements were performed.The children ranged in age from 1 to 82 months, and 145 were males. The largest calculus was 33 mm in diameter. X-ray diffraction pattern of the calculi displayed two diffraction peaks at 10.9° and 27.7° (2θ). Surgical management was performed in 14 patients. In 226 patients without surgical management, the calculi were passed in 59.63% patients within 1 month, in 85.40% within 6 and in 91.15% within 24 months. Increased SCr and urea levels were noted in three and six patients, respectively, at the time of diagnosis. The SCr, serum β2-MG, and Cys C levels at the time of diagnosis were higher than those at 3 and 6 months after diagnosis (P0.05, respectively). The levels of mALB/UCr, NAG/UCr, and RBP/UCr at the time of diagnosis were higher than those at 3, 6, 12, and 24 months after diagnosis (P0.05, respectively). α1-MG/UCr and β2-MG/UCr levels at the time of diagnosis were similar to those at 3 months after diagnosis, and significantly higher than those in the follow-up period (P0.05, respectively).Melamine might injure both the renal glomerulus and the tubule, and that the predominant lesion is urolithiasis. The compositions of melamine-induced urolithiasis are melamine and cyanuric acid crystals. The urolithiasis might persist for over 2 years and cause irreversible damage. Therefore, a long-term follow-up for all patients is required.

Polyaniline (PANI) nanowire electrodes were successfully synthesized by electrodeposition using starch as template. The electrodes were characterized with scanning electron microscope (SEM) and X-ray diffraction technique. SEM images showed that the electrodes electrodeposited using the starch template had nanowire morphology, but the PANI electrodeposited in absent solution had agglomerate block morphology. Cyclic voltammograms at different scan rates and charge–discharge tests were performed in 0.5 M H 2 SO 4 aqueous solution. The PANI nanowire electrodes had a high capacitance (882 F g − 1 ) and a high stability (5% capacity loss after 500 cycles).

Eu-doped aluminum nitride phosphors were successfully prepared using simple direct nitridation of a metallic aluminum and Eu

Miaomiao Zhang,1,* Huixiang Ju,2,* Li Zhang,1,* Mingzhong Sun,2 Zhongwei Zhou,2 Zhenyu Dai,3 Lirong Zhang,1 Aihua Gong,1 Chaoyao Wu,1 Fengyi Du1 1School of Medicine, Jiangsu University, Zhenjiang, People’s Republic of China; 2Department of Clinical Laboratory, Affiliated Yancheng Hospital, School of Medicine, Southeast University, Yancheng, Jiangsu, People’s Republic of China; 3Radiology Department, Affiliated Yancheng Hospital, School of Medicine, Southeast University, Yancheng, Jiangsu, People’s Republic of China *These authors contributed equally tothis work Abstract: X-ray computed tomography (CT) is the most commonly used imaging technique for noninvasive diagnosis of disease. In order to improve tissue specificity and prevent adverse effects, we report the design and synthesis of iodine-doped carbon dots (I-doped CDs) as efficient CT contrast agents and fluorescence probe by a facile bottom-up hydrothermal carbonization process. The as-prepared I-doped CDs are monodispersed spherical nanoparticles (a diameter of ~2.7 nm) with favorable dispersibility and colloidal stability in water. The aqueous solution of I-doped CDs showed wavelength-dependent excitation and stable photoluminescence similar to traditional carbon quantum dots. Importantly, I-doped CDs displayed superior X-ray attenuation properties in vitro and excellent biocompatibility. After intravenous injection, I-doped CDs were distributed throughout the body and excreted by renal clearance. These findings validated that I-doped CDs with high X-ray attenuation potency and favorable photoluminescence show great promise for biomedical research and disease diagnosis. Keywords: carbon dots, contrast agents, iodine-doped, CT imaging

Using D311 resin as a template, porous nano-calcium titanate microspheres (PCTOM) were prepared by a citric acid complex sol-gel method and characterized by X-ray diffraction (XRD), SEM and FTIR. The method's adsorption capabilities for heavy metal ions such as lead, cadmium and zinc were studied and adsorption and elution conditions were investigated. Moreover, taking the cadmium ion as an example, the thermodynamics and kinetics of the adsorption were studied. The results show that the microspheres were porous and were made of perovskite nano-calcium titanate. The lead, cadmium and zinc ions studied could be quantitatively retained at a pH value range of 5-8. The adsorption capacities of PCTOM for lead, cadmium and zinc were found to be 141.8 mg g(-1), 18.0 mg g(-1) and 24.4 mg g(-1) respectively. The adsorption behavior followed a Langmuir adsorption isotherm and a pseudo-second-order kinetic model, where adsorption was an endothermic and spontaneous physical process. The adsorbed metal ions could be completely eluted using 2 mol L(-1) HNO(3) with preconcentration factors over 100 for all studied heavy metal ions. The method has also been applied to the preconcentration and FAAS determination of trace lead, cadmium and zinc ion in water samples with satisfactory results.

Third generation solid dispersions (SDs) of ferulic acid (FA) in composite nanofibers were prepared using electrospinning. The spinning liquids involved co-dissolving solutions of FA, polyvinylpyrrolidone (PVP), sodium dodecyl sulfate (SDS) and sucralose in 75% ethanol aqueous solutions. FESEM observations showed that the nanofibers were assembled in a homogeneous web structure that had a smooth cross-section and surface with an average diameter of 254 ± 32 nm. Results from DSC and XRD suggested that FA, SDS and sucralose were distributed in the PVP fibers in an amorphous manner and this is due to their compatibility resulting through a second-order interactions, as demonstrated by ATR-FTIR spectra. In vitro dissolution and permeation tests showed that the nanofiber-based SDs could release all the contained FA within 1 min and had a 13-fold higher permeation rate across sublingual mucosa compared to crude FA particles. The casting films have the same compositions as the nanofibers and belong to the third generation SDs, they gave the same solubility of FA as the nanofibers, and also exhibited a much faster dissolution rate than pure FA particles. It felt that electrospinning can be taken to prepare new generation SDs with structural characteristics that enhancing absorbance of poorly soluble drugs.

Porous scaffolds of biphasic calcium phosphate (BCP)/polyamide 6 (PA6) with weight ratios of 30/70, 45/55, and 55/45 have been fabricated through a modified thermally induced phase separation technique. The chemical structure properties, macrostructure, and mechanical strength of the scaffolds were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and mechanical testing. The results indicated that the BCP/PA6 scaffolds had an interconnected porous structure with a pore size mainly ranging from 100 to 900 μm and many micropores on the rough pore walls. The mechanical property of the scaffold was significantly enhanced by the addition of BCP inorganic fillers. The 55/45 BCP/PA6 composite scaffold with 76.5% ± 2.1% porosity attained a compressive strength of 1.86 ± 0.14 MPa. Moreover, the BCP/PA6 porous scaffold was cultured with rat calvarial osteoblasts to investigate the cell proliferation, viability, and differentiation function (alkaline phosphatase). The type I collagen expression was also used to characterize the differentiation of rat calvarial osteoblasts on BCP/PA6 composite scaffold by immunocytochemistry. The in vitro cytocompatibility evaluation demonstrated that the BCP/PA6 scaffold acted as a good template for the cells adhesion, spreading, growth, and differentiation. These results suggest that the BCP/PA6 porous composite could be a candidate as an excellent substitute for damaged or defect bone.

In the present study, a calcium carbonate and calcium oxide loaded nano-hydroxyapatite/chitosan bone cement was developed and its in vitro cell responses were investigated. The physico-chemical properties were represented in terms of setting time, compressive strength, and wettability. The results show that the setting time is about 15 min, the compressive strength is up to 17.80 ± 0.45 MPa throughout the immersion period, and the static contact angle of the cement against water is 33.5° ± 2.7°, indicating that the cement has good setting time, compressive strength, and wettability. Cytocompatibility test using human MG63 cells reveals a favorable cell viability and increased proliferation over a period of 11 days in culture. The composition and hydrophilic nature of the cement provide a friendly environment for the attachment and growth of cells. The novel composite bone cement could be useful in moderate stress-bearing applications of bone repair. © 2008 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2009

Investigation of the roots of Myrica nana afforded five new cyclic diarylheptanoids, myricananins A-E (1-5), two new artifacts of myricananins A and B (6-7), and four known compounds, 12-hydroxymyricanone (8), alnusonol (9), myricatomentogenin (10), and actinidione (11). The structures of these new compounds were established by detailed spectroscopic methods. The stereochemistry of compounds 1 and 2 were determined by single-crystal X-ray diffraction. In exception of compounds 2, 6 and 10, all the other compounds were examined for their inhibitory effects on nitric oxide production in lipopolysaccharides-activated macrophages. Compounds 1, 3, 7, 8 and 9 inhibited the release of nitric oxide with IC(50) values of 45.32, 63.51, 52.81, 30.19 and 46.18 mu M, respectively. Furthermore, compound 1 was found to inhibit the expression of inducible nitric oxide synthase. (C) 2008 Elsevier Ltd. All rights reserved.

Contains fulltext : 70891.pdf (Publisher’s version ) (Open Access) Nanohydroxyapatite (n-HA)/zinc oxide (ZnO) complex was synthesized by a direct precipitation method, and the antibacterial capability and antibacterial mechanism of this complex were investigated in this article. Transmission electron microscope (TEM), Fourier transform infrared, X-ray photoelectronic spectroscopy (XPS), and X-ray diffraction (XRD) were used to analyze the materials. In addition, the antibacterial capacity of n-HA/ZnO complex was examined by bacteriolytic plate, inhibition effect, and antibacterial rate assays under light or without light. Furthermore, agarose gel electrophoresis of plasmid DNA (pUC18) was used to study biocidal action of this complex. The results of TEM observation revealed that the complex's rods had a single crystalline obelisk-like hexagonal wurtzite structure and the crystal retained the nanometer size. XRD analysis indicated that the phase of ZnO appeared and the lattice parameters of n-HA and ZnO changed. XPS spectra showed that the bonding energy of Ca, P, and O atoms changed in the complex. The analyses also showed that the two phases of ZnO and n-HA combined closely. Further, the results of the antibacterial test revealed that this complex possessed strong antibacterial capability; the antibacterial rate was 99.45% to S. aureus and 95.65% to E. coli under light, respectively. The antibacterial activity of this complex under light was better than without light, which was attributed to the generation of .OH under light. From the agarose gel electrophoresis, the dissolving solution of this complex could catalyze the cleavage of pUC18.

Nano-hydroxyapatite (n-HA)/chitosan (CS)/konjac glucomannan (KGM) composite was prepared by coprecipitation method and investigated by thermal gravitivity/differentiate thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, inductively coupled plasma emission spectroscopy, scanning electron microscopy, and energy dispersive X-ray analyzer. The analyses showed that the three phases of n-HA, CS, and KGM combined closely to each other. Further, in vitro tests were conducted to investigate the degradation and bioactivity of the composite. During immersion in simulated body fluid (SBF), pores appeared and a new substance containing Ca and P formed on the surface of the composite. Also, the concentration of Ca and P in SBF changed and weight loss of the composite was observed during time. The composite revealed a high degradation in SBF. Evidently, the new composite has a potential to be used as a carrier of implantable drug delivery system. The biodegradation rate and route could be different from CS and KGM, which will provide an opportunity to control the degradation rate or drug releasing rate by simply adjusting the ratio of CS and KGM.

A nano-hydroxyapatite (HA) coating with appropriate thickness and morphology similar to that of human bone tissue was directly prepared onto the surfaces of carbon fibers (CFs). A mixed solution of nitric acid, hydrochloric acid, sulfuric acid, and hydrogen peroxide (NHSH) was used in the preparation process. The coating was fabricated by combining NHSH treatment and electrochemical deposition (ECD). NHSH treatment is easy to operate, produces rapid reaction, and highly effective. This method was first used to induce the nucleation and growth of HA crystals on the CF surfaces. Numerous O-containing functional groups, such as hydroxyl (-OH) and carboxyl (-COOH) groups, were grafted onto the CF surfaces by NHSH treatment (NHSH-CFs); as such, the amounts of these groups on the functionalized CFs increased by nearly 8- and 12-fold, respectively, compared with those on untreated CFs. After treatment, the NHSH-CFs not only acquired larger specific surface areas but retained surfaces free from serious corrosion or breakage. Hence, NHSH-CFs are ideal depositional substrates of HA coating during ECD. ECD was successfully used to prepare a nano-rod-like HA coating on the NHSH-CF surfaces. The elemental composition, structure, and morphology of the HA coating were effectively controlled by adjusting various technological parameters, such as the current density, deposition time, and temperature. The average central diameter of HA crystals and the coating density increased with increasing deposition time. The average central diameter of most HA crystals on the NHSH-CFs varied from approximately 60 nm to 210 nm as the deposition time increased from 60 min to 180 min. Further studies on a possible deposition mechanism revealed that numerous O-containing functional groups on the NHSH-CF surfaces could associate with electrolyte ions (Ca(2+)) to form special chemical bonds. These bonds can induce HA coating deposition and improve the interfacial bonding strength between the HA coating and NHCH-CFs. The results of this study and the proposed preparation of uniform and dense nano-HA coating provide theoretical and practical guidance for future investigations of active HA coatings on fiber materials for medical products and implants. This work also lays the foundation for the wider use of HA-coated CFs/HA composite implants in clinical application.

A novel brain targeting drug delivery system based on OX26 antibody conjugation on PEGylated cationic solid lipid nanoparticles (OX26-PEG-CSLN) was prepared.The Baicalin-loaded PEGylated cationic solid lipid nanoparticles modified by OX26 antibody (OX26-PEG-CSLN) were prepared by emulsion evaporation-solidification at low temperature method. The immune-gold labeled OX26-PEG-CSLN was visualized by transmission electron microscopy. The mean diameter and zeta potential of OX26-PEG-CSLN, PEG-CSLN and CSLN were determined using a Zetasizer. The entrapment efficiency of OX26-PEG-CSLN, PEG-CSLN and CSLN was determined by ultrafiltration centrifugation method. And the solid-state characterization of OX26-PEG-CSLN and CSLN were analyzed by X-ray. Pharmacokinetics studies were conducted by in vivo microdialysis in rat cerebrospinal fluid.The results showed that the OX26-PEG-CSLN, PEG-CSLN and CSLN had average diameters of 47.68 ± 1.65, 27.20 ± 1.70 and 33.89 ± 5.74 nm, Zeta potentials of -0.533 ± 0.115 mV, 11.200 ± 0.500 mV and 11.080 ± 1.170 mV and entrapment efficiencies of 83.03 ± 0.01%, 92.90 ± 3.50% and 97.83 ± 0.19%, respectively. In the pharmacokinetics studies, the AUC value of OX26-PEG-CSLN was11.08-fold higher than that of the Baicalin solution (SOL) (p0.01), and 1.12-fold higher than that of the CSLN (p0.05); the Cmax value of OX26-PEG-CSLN was 7.88-fold higher than that of SOL (p0.01) and 1.12-fold (p0.01) higher than that of the CSLN, respectively.These results demonstrated OX26-PEG-CSLN could be a promising carrier to deliver drugs across the BBB for the treatment of brain diseases.

Five new ent-kaurane diterpenoids, ludongnins F-J (1-5), along with 10 known compounds, guidongnins A-C (6-8), angustifolin (9), 6-epiangustifolin (10), sculponeatin J (11), gardenin D, 5,3',4'-trihydroxy-6,7,8-trimethoxyflavone, pedalitin, and quercetin, were isolated from the leaves of Isodon rubescens var. lushiensis. The structures of 1-5 were determined by spectroscopic analysis, as well as X-ray crystallographic analysis of 1. Compounds 1-11 were evaluated against K562 leukemia cells for their cytotoxic effects.

High performance magnetic Fe3O4/PAH/PSS@Pd core-shell microspheres are successfully synthesized via layer-by-layer self-assembly method. Fe3O4 cores with a rough surface are synthesized by hydrothermal method. Subsequently, Pd nanoparticle shells and Fe3O4/PAH/PSS@Pd microspheres are in situ simultaneously constructed by alternating immersion of Fe3O4 particles in PSS (poly(sodium 4-styrenesulfonate)) and PAH-Pd(II) (Poly(allylamine hydrochloride)-Pd(II)) solutions, followed by chemical reduction in NaBH4 solution. The structural and magnetic properties of microspheres are characterized by transmission electron microscopy (TEM), scanning electron microscope (SEM), X-ray diffraction analysis (XRD), and vibrating sample magnetometer (VSM), respectively. These microspheres demonstrate excellent structural uniformity (190nm) and superior magnetization, leading to easy collection of microspheres using an external field. With highly active and stable Pd nanoparticle shells, these microspheres exhibit more efficient catalytic activity for the oxidation of benzyl alcohol.

The silver cube-like nanostructure with uniform size and high yield have been synthesized through the rapid sulfide-mediated polyol method. The morphology, structure and optical properties of the as-prepared silver nanocubes were characterized by UV-Visible spectroscopy, field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The Surface-Enhanced Raman Scattering (SERS) performance of the as-prepared Ag nanocubes was characterized by crystal violet (CV) as the probe molecules. Furthermore, the low levels of thiram and pesticide paraoxon can be detected by the SERS technique, which shows that the silver nanocubes as a SERS substrate have excellent sensitivity and reproducibility.

Toxicodenanes A-C (1-3), representing sesquiterpenoids with three new carbon skeletons, were isolated from the dried resin of Toxicodendron vernicifluum. Their structures were identified by spectroscopic data and X-ray diffraction crystallography. Their plausible biosynthetic route was proposed via the isolated intermediate (4). Compounds 2 and 3 could significantly inhibit overproduction of fibronectin, collagen IV, and IL-6 in high-glucose-induced mesangial cells in a dose- and time-dependent manner, showing their potential in diabetic nephropathy.

The crystal structure of a recombinant form of the proteinase encoded by the feline immunodeficiency virus (FIV PR) has been solved at 2 A resolution and refined to an R-factor of 0.148. The refined structure includes a peptidomimetic, statine-based inhibitor, LP-149, which is an even more potent inhibitor of HIV PR. Kinetic parameters were obtained for the cleavage of five substrates by FIV PR, and inhibition constants were measured for four inhibitors. The structure of FIV PR resembles other related retroviral enzymes although few inhibitors of HIV PR are capable of inhibiting FIV PR. The structure of FIV PR will enhance our knowledge of this class of enzymes, and will direct testing of new proteinase inhibitors in a feline animal model.

Two kinds of amino groups were employed to functionalize bimodal mesoporous silicas and related drug carriers were prepared. The characterization results of XRD, N2 adsorption and desorption, FT-IR and TG all confirmed the structural integrity of the bimodal mesopore architecture after introduction treatment of functional groups and the successful adsorption of aspirin. In order to investigate the interaction among the mesoporous structure, the functional groups grafted onto the mesoporous surface and the existential microenvironment of the drug molecules inside the mesoporous channels, the thermal decomposition behaviors of amino groups modified and aspirin loaded carriers were studied based on the thermogravimetric analysis in details. According to the thermogravimetry and derivative thermogravimetry results, the apparent activation energies E(a) of thermal decomposition for all related samples have been evaluated by Kissinger and Flynn-Wall-Ozawa methods. Meanwhile, their thermal decomposition mechanisms have been suggested by using Coats and Redfern methods. All these featured consequence could provide a deeper understanding for large loading capacity and controlled release of drug-carriers in the pharmaceutical application.

The synthesis of modified bimodal mesoporous materials (BMMs) with a small pore size of around 2.9 nm and a large pore size of about 20 nm has been performed via post-grafting methods. To study the application of functionalized BMMs in drug delivery, loading and releasing profiles using aspirin as model drug were carried out. XRD, SEM, TEM, N2 adsorption, FT-IR, 29Si-NMR, TG and UV-Vis spectroscopy were used to characterize the related samples. The post-grafting modification was performed through the weak chemical interaction or hydrogen bonding in between OH groups of the mesopore surface and 3-aminopropyltriethoxysilane (N-TES) or 3-(2-aminoethylamino) propyItrimethoxysilane (NN-TES). The results showed that N-TES groups with different amount and NN-TES groups were successfully incorporated onto the mesopore surface. Subsequently, the controlled aspirin delivery properties from the resulting modified BMMs were investigated in detail. The aspirin adsorption experiments indicated that the adsorption capacities of modified BMMs were improved with the increasing amount of N-TES groups, while the NN-TES functionalized samples showed higher adsorption capacity than N-TES modified samples with the same ratio of modification. The most reason is that the interaction between the NN-TES groups and aspirin molecules is stronger than that between the N-TES groups and aspirin molecules. The in vitro tests exhibited that aspirin release behaviors mainly depended on the variation of the amount and species of the functional groups in mesoporous carries. According to the Korsmeyer-Peppas model, it is found that the kinetic release constant k reduced with the increase amount of the amino groups on the mesopore surface of modified BMMs, suggesting that the aspirin release rate from the pores of BMMs was influenced directly by organic groups on the surface. The release exponent n of all the situations were above 0.5, indicating the drug release mechanism followed a non-Fickian model that was diffusion based. Therefore, this type of materials described in this paper is of strong potential for the controlled drug release applications.

Self-assembly of several low-molecular-weight L-glutamic acid-based gelators, which individually formed helical nanotube or nanofiber structures, was investigated in the presence of Cu(2+) ion. It was found that, when Cu(2+) was added into the system, the self-assembly manner changed significantly. Only in the case of bolaamphiphilic glutamic acid, N,N'-hexadecanedioyl-di-L-glutamic acid (L-HDGA), were the hydrogel formation as well as the nanotube structures maintained. The addition of Cu(2+) ion caused a transition from monolayer nanotube of L-HDGA to a multilayer nanotube with the thickness of the tubular wall about 10 nm. For the other amphiphiles, the gel was destroyed and nanofiber structures were mainly formed. The formed Cu(2+)-containing nanostructures can function as an asymmetric catalyst for Diels-Alder cycloaddition between cyclopentadiene and aza-chalcone. In comparison with the other Cu(2+)-containing nanostructures, the Cu(2+)-mediated nanotube structure showed not only accelerated reaction rate, but enhanced enantiomeric selectivity. It was suggested that, through the Cu(2+) mediated nanotube formation, the substrate molecules could be anchored on the nanotube surfaces and produced a stereochemically favored alignment. When adducts reacted with the substrate, both the enantiomeric selectivity and the reaction rate were increased. Since the Cu(2+)-mediated nanotube can be fabricated easily and in large amount, the work opened a new way to perform efficient chiral catalysis through the supramolecular gel.

Mesoporous TiO₂ beads with diameters of 320±50, 550±50, and 830±40 nm, comprising interconnected and densely packed TiO₂ nanocrystals, were used as working electrodes for dye-sensitized solar cells (DSCs). These electrodes possess high surface areas and superior light-scattering properties, which are ideal for DSC applications. Although the electrode prepared by using 320±50 nm beads demonstrated the highest dye loading and the electrode prepared by using 550±50 nm beads showed the best light-scattering properties in the wavelength region λ=400-800 nm, DSC devices with working electrodes composed of 830±40 nm beads achieved the highest power conversion efficiencies of 9.0 % after treatment with TiCl₄. A higher electron diffusion rate (4.35×10⁻⁴ cm² s⁻¹) and an extended electron lifetime (58 ms) were observed in DSCs composed of the largest beads, 830±40 nm, attributable to a reduced amount of inter-bead barriers and a relatively small percentage of TiO₂ nanocrystals on the surface of the beads, compared to cells containing 550±50 and 320±50 nm beads.

This paper employs methods used earlier to study helix propensity in a model α-helix. The methods are extended to simulations of a motif structure of the α-helical coiled coil, i.e., a structure with a simple amino acid sequence, containing only alanine, leucine, and valine, with leucine and valine forming hydrophobic contacts in the helix interface (positions “d” and “a”). Dynamic simulations of the model coiled-coil structure reproduce characteristic features of the coiled-coil motif seen in experimental studies. Free energy simulations were used to assess the change in stability of the model when a leucine pair or a valine pair in the helix interface was replaced with an alanine pair. A leucine pair at position d was found to contribute 3.4 kcal/mol to the stability of the coiled coil relative to an alanine pair, and a valine pair at postion a was found to contribute 0.8 kcal/mol relative to an alanine pair. The value for the leucine pair agrees with reports in two experimental studies with molecules having different amino sequence. The value for the valine pair is reasonable given the smaller size of the valine side chain and the intrinsic low helix propensity of valine. No experimental value was available for comparison. © 1993 Wiley-Liss, Inc.

High-resolution hard X-ray grating-based imaging method with conventional X-ray sources provides attenuation, refraction and scattering information synchronously, and it is regarded as the next-generation X-ray imaging technology for medical and industrial applications. In this letter, a large phase-stepping approach with at least one order of magnitude lower resolution of the movement is presented to equivalently substitute the current high-positioning-resolution phase-stepping approach. Both the theoretical deduction and actual experiment prove that the new approach is available to relax the requirement of high positioning resolution and strict circumstances so as to benefit the future commercial applications of the grating-based multiple-information imaging technology.

Different concentrations of berberine were mixed with nano-hydroxyapatite/chitosan (n-HA/CS) bone cement to generate an antibiotic drug delivery system for treatment of bone defects. Properties of the system such as setting time, compressive strength, surface morphology, phase compositions, drug release profiles and antimicrobial activity were also characterized. It was shown that the setting time of the cement ranged from 17.03 +/- 0.50 min to 28.47 +/- 0.96 min and the compressive strength changed from 184.00 +/- 7.94 MPa to 120.33 +/- 9.02 MPa with the increase of berberine. The XRD, IR, and SEM analyses suggested that berberine powders were stable in the bone cement in simulated body fluid (SBF). In vitro release of berberine from the bioactive bone cement pellets in SBF could last more than 4 weeks. The release profiles of 1.0 wt % berberine loaded bone cement followed the Higuchi equation at the infusion stage. The drug loaded pellets can inhibit bacterial growth (Staphylococcus aureus) at the standardized berberine minimum inhibitory concentration of 0.02 mg/mL during berberine release from 1 to 28 days. The n-HA/CS bone cement only with 1.0 wt % berberine proved to be an efficient antibiotic drug delivery system.

Controlling the process of crystal growth is of importance to the biomineralization and materials science. In this work, some novel morphology of calcium carbonate (CaCO3) was precipitated in an ethanol-water binary solvent (EWBS) with a CaCl2/Na2CO3 reaction system. For the solutions of CaCl2/Na2CO3 in EWBS, the alcoholization and hydration of Ca2+ and CO3(2-) were discussed from the radial distribution functions by molecular dynamics simulations, and the number density profiles of water molecules around and approximately 15 A away from CO3(2-) were employed to reveal the distribution of water molecules. It is found that EWBS has a divisive effect on Ca2+ and CO3(2-), and the local inhomogeneity of EWBS would be enhanced by adding some Na2CO3 into it. This inhomogeneity results in an aqueous two-phase system as x E goes up to 0.7. In addition, the novel morphology of CaCO3 under different molar ratios of Ca2+/CO3(2-) and in different mixed solvents were confirmed by XRD and SEM, and the relationships between the morphology of CaCO 3 and the structural properties of mixed solvents were further explored.