Synchrotron radiation X-ray fluorescence analysis of Fe, Zn and Cu in mice brain associated with Parkinson's disease

The contents and distributions of metal elements in the brain are closely related to neurodegenerative diseases.In this study, we examined Fe, Cu and Zn contents in the brain section associated with Parkinson‘s disease(PD)using synchrotron radiation X-ray fluorescence(SRXRF). PD mouse model induced by 1-methyl-4-phenyl-1,2,3,6-terahydropyridine(MPTP) was used for the elemental analysis(e.g., Fe, Cu and Zn) in the substantia nigra pars compacta(SNpc) region of mice brain tissue samples. We found that mice in the MPTP group had higher contents of Fe, Cu and Zn in the SNpc than the control group. After treating the PD mice with rapamycin, the contents of Fe, Cu and Zn were reduced, the dopamine neurons and motor function were rescued correspondingly. The results prompted that the SRXRF provided an ideal method for tracing and analyzing the metal elements in the brain section to assess the pathological changes of PD model and the therapeutic effect of drugs.

Synchrotron radiation X-ray fluorescence analysis on altered mineral muscovite in gold deposit

Synchrotron radiation X-ray fluorescence (SRXRF) microprobe was used to ananlyse altered mineral muscovite and its surrounding feldspar in Yuerya gold deposit. The major, minor and trace elements of the two minerals were detected and analyzed. SRXRF analysis showed that the Yuerya muscovite had a complex chemical composition, containing K, Fe, Ca, Ti, Cr, Mn, Co, Cu, Zn and many trace or ultra-trace elements. Since muscovite resulted from the alteration of hydrothermal ore fluid acting on feldspar (plagioclase), the difference of chemical composition between the two minerals shows the components of ore fluid, which are characterized by the enrichment of alkaline and alkaline-earth metal elements K, Ca and ore-associated elements Fe, Cu, Zn. And gold, silver and platinum, invisible under microscope, were detected in some areas of muscovite, but not found in feldspar. Espe- cially platinum, a mantle material, is rarely seen in the earth crust but now found in the gold deposit of magmatic sources; its appearance approves the idea of mantle flux participating in the gold mineralization, which suggests that the tectonic event controlling gold mineralization in the Yuerya district is a mantle phenomenon.

L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

Operando measurement of lattice deformation profiles of synchrotron radiation monochromator

This study presents a new method for characterizing the thermal lattice deformation of a monochromator with high precision under service conditions and first reports the operando measurements of nanoscale thermal lattice deformation on a double-crystal monochromator at different incident powers.The nanoscale thermal lattice deformation of the monochromator first crystal was obtained by analyzing the intensity of the distorted DuMond diagrams.DuMond diagrams of the 333 diffraction index,sensitive to lattice deformation,were obtained directly using a 2D detector and an analyzer crystal orthogonal to the monochromator.With increasing incident power and power density,the maximum height of the lattice deformation increased from 3.2 to 18.5 nm,and the deformation coefficient of the maximum height increased from 1.1 to 3.2 nm/W.The maximum relative standard deviation was 4.2%,and the maximum standard deviation was 0.1 nm.Based on the measured thermal deformations,the flux saturation phenomenon and critical point for the linear operation of the monochromator were predicted with increasing incident power.This study provides a simple solution to the problem of the lower precision of synchrotron radiation monochromator characterizations compared to simulations.

Analysis of nickel distribution by synchrotron radiation X-ray fluorescence in nickel-induced early- and late-phase allergic contact dermatitis in Hartley guinea pigs

Background: Nickel-induced allergic contact dermatitis (Ni-ACD) is a global health problem. More detailed knowledge on the skin uptake of haptens is required. This study aimed to investigate the penetration process and distribution of nickel in skin tissues with late phase and early phase of Ni-ACD to understand the mechanisms of metal allergy. Methods: Forty Hartley guinea pigs were divided into four groups according to the NiSO4 sensitizing concentration and the NiSO4 challenged concentration: the 5% NiSO4-group, 5% to 10%(sensitization-challenge;late phase group);10% NiSO4-group, 10% to 10%(sensitization-challenge;early-phase group);and the positive and negative controls. Pathological biopsies were performed on each group. The depth profile of nickel element concentration in the skin of guinea pigs was detected by synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μ-XRF) and micro X-ray absorption near-edge spectroscopy (μ-XANES). Results: In each section, the nickel element concentration in both the 5% NiSO4-group and 10% NiSO4-group was significantly higher than that in the negative control group. In the upper 300-μm section of skin for the early phase group, the nickel element concentration was significantly higher than that in the lower section of skin. In deeper sections (>200 μm) of skin, the concentration of nickel in the early phase group was approximately equal to that in the late phase group. The curve of the late phase group was flat, which means that the nickel element concentration was distributed uniformly by SR-μ-XRF. According to the XANES data for the 10% NiSO4 metal salt solution, structural changes occurred in the skin model sample, indicating that nickel was not present in the Ni^2+ aqueous ionic state but in the nickel-binding protein. Conclusions: This study showed that the distribution of the nickel element concentration in ACD skin tissue was different between the early phase and late phase groups. The nickel element was not present in the Ni^2+ aqueous ionic state but bound with certain proteins to form a complex in the stratum corneum in ACD model tissue.

In situ analysis of trace elements in metalloproteins of human liver by synchrotron radiation X-ray fluorescence

A method using synchrotron radiation X-ray fluorescence analysis toin situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed along polyacrylamide gel. The results showed that the protein fraction of peak III in cytosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique forin situ analysis of trace elements in protein bands.

Characterization of metal element distributions in the rat brain following ischemic stroke by synchrotron radiation microfluorescence analysis

Ischemic stroke is one of the leading causes of death worldwide,and effective treatment strategies in the chronic phase of this disease remain insufficient.Homeostasis of metals in the brain plays an important role in maintaining normal brain function.However,the dynamic spatial distributions of iron,zinc,calcium,potassium,and copper in a rat brain following ischemic stroke and the association between structural distribution and function remain to be elucidated.In this study,we used a synchrotron radiation-based micro-X-ray fluorescence technique to image element mapping changes in special rat brain regions after ischemic stroke,showing the distribution characteristics of iron,zinc,calcium,potassium,and copper.We demonstrated,for the first time,the consistent dynamic spatial distributions of metal elements at a series of time points(3 h,4.5 h,6 h,12 h,1 d,3 d,5 d,7 d,10 d,14 d,28 d)after brain ischemia,which revealed that the homeostasis of iron,zinc,calcium,potassium,and copper in the brain was disturbed with distinctive change trends,providing clear insights in understanding the underlying pathogenesis of stroke from a novel perspective,thus laying the foundation of further developing new drug targets for stroke treatment.

Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

Scanning Analysis of REE in Bastnaesite with Synchrotron Radiation X－Ray Fluorescence Microprobe

The content of REE(La.Ce.Pr.Nd.Sm) in bastnaesite was measured by synchrotron radiation X-ray fluorescence microprobe.Scanning analysis makes use of excitation of the REE K lines between 33 and 50 keV.SR white beam from a Wiggler source at the Beijing Electron Positron Collider(BEPC) of the National Laboratory,in order to excite the REE.The bastnaesite from the same mineral area was powdered to particle size≤300 mesh.It was then divided into two parts.One portion was used to be determined by XRF after depositing with oxalate and transforming into oxide.The other was pressed into disk without any binder as the reference sample.The weight and the diamieter of the disk were 15 g and 26 mm respectively.

Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time. The butterfly-wings scattering patterns are composed of several branches. The angles between the branches are roughly equal to that between the habit planes of precipitates. The evolution of Guinier radius with aging time indicates the good coarsening resistance of the precipitates. The evolution of integrated intensity is consistent with the classical two-step precipitation process.

Polycapillary X-ray lens for the secondary focusing Beijing synchrotron radiation source

According to intensity distribution of the synchrotron radiation source focused by a toroidal mirror at the Beijing synchrotron radiation biological macromolecule station, theoretical modeling of the Beijing synchrotron radiation source is developed for capillary optics. Using this theoretical modeling, the influences of the configuration curve of the polycapillary X-ray lens on transmission efficiency and working distance are analyzed. The experimental results of the transmission efficiency and working distance at the biological macromolecule station are in good agreement with the theoretical results.

Internal Structure of Cambrian Fossil Embryo Markuelia Revealed in the Light of Synchrotron Radiation X-ray Tomographic Microscopy

In the light of Synchrotron Radiation X-ray Tomographic Microscopy （SRXTM）, the internal structure of Markuelia hunanensis is revealed. In one example, vitrification and peeling show the annuli hidden under the chorion. Sectioning and 3-D reconstruction display an intact digestive tract from the inverted introvert to the terminal anus. The inverted introvert forms a rugby cavum. The following digestive tract is rope-like coiling, parallel to the body axis, about 650 μm in length, and uniform in diameter （-80 μm）. An exquisitely preserved pipe-like structure is hidden in the middle of the rope-like structure, diameter 20--40 lam, with a length of -120 μm. We interpret this pipe-like structure as the possible epidermis of the gut and its surroundings as the possible residue of musculature, similar to that in Priapulans. The two symmetrical rod-shape structures connecting the body wall and digestive tract are interpreted as the possible retractor muscles. After comparing the well preserved Left-form and Right-form Body of Markuelia, we suggest that they may represent a dimorphism. Counted directly, one sample of Markuelia hunanensis possesses 62 annulations and the other 68.

Three dimensional distribution of surfactant in microspheres revealed by synchrotron radiation X-ray microcomputed tomography

This study investigated the formulation mechanism of microspheres via internal surfactant distribution. Eudragit L100 based microspheres loaded with bovine serum albumin were prepared by solid in oil in oil emulsion solvent evaporation method using acetone and liquid paraffin system containing sucrose stearate as a surfactant. The fabricated microspheres were evaluated for encapsulation efficiency, particle size, production yield, and in vitro release characteristics. The internal structures of microspheres were characterized using synchrotron radiation X-ray microcomputed tomography(SR-μCT). The enhanced contrast made the sucrose stearate distinguished from Eudragit to have its three dimensional(3D) distribution. Results indicated that the content and concentration determined the state of sucrose stearate and had significant influences on the release kinetics of protein. The dispersity of sucrose stearate was the primary factor that controlled the structure of the microspheres and further affected the encapsulation efficiency, effective drug loading, as well as in vitro release behavior. In conclusion, the 3D internal distribution of surfactant in microspheres and its effects on protein release behaviors have been revealed for the first time. The highly resolved 3D architecture provides new evidence for the deep understanding of the microsphere formation mechanism.

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction（XRD） in diamond anvil cells（DACs） using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF（Beijing Synchrotron Radiation Facility） and some results are also presented.

Preliminary determination of calcium,phosphorus,and the calcium/phosphorus ratio in cortical bone of Chinstrap penguin using synchrotron X-ray fluorescence analysis

Synchrotron radiation X-ray fluorescence （SR-XRF） approach was applied to analyzing of Chinstrap penguin （ Pygoscelis Antarctica） cortical bone. The method enabled the in situ determination of Ca and P concentrations and the Ca/P ratio in cortical bone. The preliminary results show that ： （ 1 ） there is the bone site-related difference for Ca and P concentrations. The mean values for the investigated parameters （ on a dry-weight basis） are： 30.7% （Ca） and 14.9% （P） for the femoral cortical bone, 21.4% （Ca） and 11.5% （P） for wing cortical bone. （2） The variation for the Ca/P ratio in cortical bone is lower than those for Ca and P separately. This is in agreement with the previous report that the specificity of the Ca/P ratio is better than that of Ca and P concentrations and is more reliable for the diagnosis of bone disorders. The authors suggest that further studies be conducted to establish norreal values of Ca, P and Ca/P ratio for polar animals and provide a basis for the diagnosis of bone disorders.

The Study Internal Structure of the Annual Layers in Lake Sediments Using Synchrotron Radiation with X-ray Focusing Optics

1 Introduction Annually laminated(varve)sedimentary deposits are considered as one of the most important archives,since they offer precise temporal information(years)in combination with high time resolutions.Bottom sediments of the lakes contain detailed geochemical information on

Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radia- tion Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2~=t=0.25 ~_ （11=0.1 nm） which is co- incident with other ones＇ results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed.

Hard X-ray in-line outline imaging for blood vessels:first generation synchrotron radiation without contrast agents in vitro

Objective: Phase-contrast X-ray imaging which reduces radiation exposure, is a promising technique for observing the inner structures of biological soft tissues without the aid of contrast agents. The present study intends to depict blood vessels of rabbits and human livers with hard X-ray in-line outline imaging without contrast agents using synchrotron radiation. Methods: All samples were fixed with formalin and sliced into 6 mm sections. The imaging experiments were performed with Fuji-IX80 films on the 4W1A light beam of the first generation synchrotron radiation in Beijing, China. The device of the experiment, which supplies a maximum light spot size of 20×10 mm was similar to that of in-line holography. The photon energy was set at 8 KeV and high quality imagines were obtained by altering the distance between the sample and the film. Results: The trees of rabbit-liver blood vessels and the curved vessels of the cirrhotic human liver were revealed on the images, where vessels < 20 μm in diameter were differentiated. Conclusion: These results show that the blood vessels of liver samples can be revealed by using hard X-ray in-line outline imaging with the first generation synchrotron radiation without contrast agents.

Focusing high-energy x-rays by a P MMA compound x-ray lens on Beijing synchrotron radiation facility

The x-ray compound lens is a novel refractive x-ray optical device. This paper reports the authors＇ recent research on a polymethyl methacrylate （PMMA） compound x-ray lens. Firstly the designing and LIGA fabrication process for the PMMA compound x-ray lens are briefly described. Then, a method for theoretical analysis, as well as the experimental system for measurement is also introduced. Finally, the focusing spots for 8keV monochromatic x-rays by the PMMA compound x-ray lens are measured and analysed. According to the experimental results, it is concluded that the PMMA compound x-ray lens promises a good focusing performance under the high-energy x-rays.

The Significance of Solutions Obtained from Ill-Posed Systems of Linear Equations Constituted by Synchrotron Radiation Based Anomalous Small-Angle X-Ray Scattering

Synchrotron radiation based experimental techniques known as Anomalous Small-Angle X-ray Scattering (ASAXS) provide deep insight into the nanostructure of uncountable material systems in condensed matter research i.e. solid state physics, chemistry, engineering and life sciences thereby rendering the origin of the macroscopic functionalization of the various materials via correlation to its structural architecture on a nanometer length scale. The techniques constitute a system of linear equations, which can be treated by matrix theory. The study aims to analyze the significance of the solutions of the stated matrix equations by use of the so-called condition numbers first introduced by A. Turing, J. von Neumann and H. Goldstine. Special attention was given for the comparison with direct methods i.e. the Gaussian elimination method. The mathematical roots of ill-posed ASAXS equations preventing matrix inversion have been identified. In the framework of the theory of von Neumann and Goldstine the inversion of certain matrices constituted by ASAXS gradually becomes impossible caused by non-definiteness. In Turing’s theory which starts from more general prerequisites, the principal minors of the same matrices approach singularity thereby imposing large errors on inversion. In conclusion both theories recommend for extremely ill-posed ASAXS problems avoiding inversion and the use of direct methods for instance Gaussian elimination.