1.Interfacial modulus mapping of layered dental ceramics using nanoindentation.
Antonios L THEOCHAROPOULOS ; Andrew J BUSHBY ; Ken MY P'NG ; Rory M WILSON ; K Elizabeth TANNER ; Michael J CATTELL
The Journal of Advanced Prosthodontics 2016;8(6):479-488
PURPOSE: The aim of this study was to test the modulus of elasticity (E) across the interfaces of yttria stabilized zirconia (YTZP) / veneer multilayers using nanoindentation. MATERIALS AND METHODS: YTZP core material (KaVo-Everest, Germany) specimens were either coated with a liner (IPS e.max ZirLiner, Ivoclar-Vivadent) (Type-1) or left as-sintered (Type-2) and subsequently veneered with a pressable glass-ceramic (IPS e.max ZirPress, Ivoclar-Vivadent). A 5 µm (nominal tip diameter) spherical indenter was used with a UMIS CSIRO 2000 (ASI, Canberra, Australia) nanoindenter system to test E across the exposed and polished interfaces of both specimen types. The multiple point load – partial unload method was used for E determination. All materials used were characterized using Scanning Electron Microscopy (SEM) and X – ray powder diffraction (XRD). E mappings of the areas tested were produced from the nanoindentation data. RESULTS: A significantly (P<.05) lower E value between Type-1 and Type-2 specimens at a distance of 40 µm in the veneer material was associated with the liner. XRD and SEM characterization of the zirconia sample showed a fine grained bulk tetragonal phase. IPS e-max ZirPress and IPS e-max ZirLiner materials were characterized as amorphous. CONCLUSION: The liner between the YTZP core and the heat pressed veneer may act as a weak link in this dental multilayer due to its significantly (P<.05) lower E. The present study has shown nanoindentation using spherical indentation and the multiple point load - partial unload method to be reliable predictors of E and useful evaluation tools for layered dental ceramic interfaces.
Ceramics*
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Elastic Modulus
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Hot Temperature
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Methods
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Microscopy, Electron, Scanning
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Powder Diffraction
2.Kinetic study on dissociation of amylose/salicylic acid compound using non-isothermal method.
Qi-fang WANG ; San-ming LI ; Xin CHE ; Chao-jie LI
Acta Pharmaceutica Sinica 2010;45(7):909-913
The inclusion compound of amylose and salicylic acid (SA) was prepared by a sealed temperature control method, and the formation of the inclusion compound was confirmed by IR spectrum and powder X-ray diffraction. The kinetic parameters of dissociation of amylose/SA compound were studied by the nonisothermal method which was defined as a relationship between the dissociation ratio and time. The values of activation energy (Ea) and frequency factors (InA) were calculated by a nonlinear least-square method. In this study, the formation of the inclusion compound of amylose/SA was confirmed by IR spectrum powder X-ray diffraction. SA existed in a molecule form in the spiral stouction of amylose. The dissociation of amylose/SA compound was attributed to first order reaction. The values of Ea calculated by the nor-isothermal method were 21.71 and 22.41 kJ x mol(-1) at heating rate 5 and 10 degrees C x h(-1), respectively. The corresponding isothermal method value of Ea was 22.17 kJ x mol(-1); the calculated InA values were 9.32 and 10.08 at heating rate 5 and 10 degrees C x h(-1), respectively. The corresponding isothermal method lnA value was 9.26. The results were in good agreement with Ea values and lnA values by isothermal method. These results indicated that the non-isothermal method described in this study could be adequately used for the stability study of inclusion compound and was a rapid and accurate method for the determination of kinetic parameters.
Amylose
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chemistry
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Drug Stability
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Hot Temperature
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Kinetics
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Powder Diffraction
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Salicylic Acid
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chemistry
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Spectrophotometry, Infrared
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Thermodynamics
3.Preparation and release behaviour of mesoporous silica/ethylcellulose sustained-release mini-matrix.
Qiao-li WU ; Gui-lan QUAN ; Yu HONG ; Lin-na WU ; You-mei ZENG ; Ge LI ; Xin PAN ; Chuan-bin WU
Acta Pharmaceutica Sinica 2015;50(4):492-499
Hot-melt extrusion was applied to prepare mesoporous silica/ethylcellulose mini-matrix for sustained release, and fenofibrate was used as a model drug, ethylcellulose and xanthan gum were chosen as sustained-release agent and releasing moderator, respectively. This novel matrix obtained the controlled release ability by combining mesoporous silica drug delivery system and hot-melt extrusion technology. And mesoporous silica particle (SBA-15) was chosen as drug carrier to increase the dissolution rate of fenofibrate in this martix. Scanning electron microscope, transmission electron microscope, small angle X-ray powder diffraction and N2 adsorption-desorption were introduced to determine the particle morphology, particle size and pore structure of the synthesized SBA-15. The results showed that SBA-15 had a very high Brunauer-Emmett-Teller specific surface area, a narrow pore size distribution, large pore volume and a ordered two-dimensional hexagonal structure of p6mm symmetry. Differential scanning calorimetry and X-ray powder diffraction results demonstrated that fenofibrate dispersed in an amorphous state inside the pores of the mesoporous silica which contributed to the improvement in the dissolution rate. The drug release of mini-matrices was influenced by ethylcellulose viscosity grades and xanthan gum concentration, which increased with the increasing of xanthan gum concentration and decreasing of ethylcellulose viscosity. Mini-matrix containing 22% xanthan gum exhibited a good sustained release performance, and the drug release behavior followed the first-order kinetics.
Adsorption
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Calorimetry, Differential Scanning
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Cellulose
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analogs & derivatives
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Delayed-Action Preparations
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Drug Carriers
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chemistry
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Particle Size
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Porosity
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Powder Diffraction
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Powders
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Silicon Dioxide
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Solubility
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X-Ray Diffraction
4.Combined analysis of urinary stones by X-ray photoelectron spectroscopy and X-ray powder diffraction.
Jian-ming OUYANG ; Xiang-ping LI
Acta Academiae Medicinae Sinicae 2003;25(6):710-713
OBJECTIVETo seek the methods in the prevention and cure of urinary stones in the Zhujiang valley in Guangdong province.
METHODSTwenty random urinary stones were quantitatively and morphologically analyzed by X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD).
RESULTSCalcium oxalate (about 70%) was the main composition of urinary stones in the Zhujiang valley in Guangdong province; while 30% of which was uric acid stones. Most calcium oxalate stones contain phosphate; however, its content usually was less than 10%.
CONCLUSIONSCalcium oxalate, uric acid and phosphate are the main compositions of urinary stones in the Zhujiang valley in Guangdong province. The compositions and phases of urinary stones can be obtained accurately by the combination of XPS and XRD.
Adult ; Aged ; Calcium Oxalate ; analysis ; Female ; Humans ; Male ; Middle Aged ; Powder Diffraction ; Spectrometry, X-Ray Emission ; methods ; Uric Acid ; analysis ; Urinary Calculi ; chemistry ; X-Ray Diffraction ; methods
5.Preparation, characterization, and in vivo evaluation of a polymorphic form of valnemulin hydrogen tartrate
Xinle ZHU ; Shixin XU ; Lianshou LU ; Shensen WANG ; Qi ZHAO ; Dan LI ; Jian LI ; Hui ZHAO ; Bingen XU
Journal of Veterinary Science 2019;20(2):e16-
We prepared a polymorphic form of valnemulin hydrogen tartrate (Form I) to overcome the instability and irritating odor of valnemulin hydrochloride that affect its use in the production and application of veterinary drugs. The physicochemical properties of Form I were characterized by scanning electron microscopy, X-ray powder diffraction, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The results showed the crystal structure and thermal properties of Form I were very different from those of a commercially available form of valnemulin hydrogen tartrate (Form II). Form I and Form II were more stable than valnemulin hydrochloride after storage under irradiation and high humidity conditions, respectively. The solubility of Form I was 2.6 times that of Form II, and Form I was selected for use in pharmaceutical kinetics experiments in vivo. Compared to valnemulin hydrochloride, after oral administration at a dose of 10 mg/kg in pigs, Form I had similar pharmaceutical kinetic behavior but a slightly higher area under the concentration–time curve from time zero to the last measurable concentration. Consequently, Form I should be suitable for the development of simple formulations and be effective in the clinical application of veterinary drugs.
Administration, Oral
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Calorimetry, Differential Scanning
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Humidity
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Hydrogen
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Kinetics
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Microscopy, Electron, Scanning
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Odors
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Pharmacokinetics
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Powder Diffraction
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Solubility
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Spectrum Analysis
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Swine
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Veterinary Drugs
6.The influence of spray drying process conditions on physical, chemical properties and lung inhaling performance of Panax notoginseng saponins - tanshinone II A composite particles.
Hua-Mei WANG ; Ting-Ming FU ; Li-Wei GUO
Acta Pharmaceutica Sinica 2013;48(6):925-932
This study is to report the influence of conditions in spray drying process on physical and chemical properties and lung inhaling performance of Panax notoginseng Saponins - Tanshinone II A composite particles. According to the physical and chemical properties of the two types of components within the composite particles, three solvent systems were selected including ethanol, ethanol : acetone (9 : 1, v/v) and ethanol : acetone (4 : 1, v/v), and three inlet temperature: 110 degrees C, 120 degrees C, 130 degrees C to prepare seven different composite particle samples; each sample was characterized using laser diffraction, scanning electron microscopy (SEM), dynamic vapour sorption (DVS) and atomic force microscope (AFM), and their aerodynamic behavior was evaluated by a Next Generation Impactor (NGI). The results indicate that under the conditions of using the mixed solvent system of ethanol--acetone volume ratio of 9 : 1, and the inlet temperature of 110 degrees C, the resulting composite particles showed rough surface, with more tanshinone II A distributing in the outer layer, such composite particles have the best lung inhaling performance and the fine particle fraction (FPF) close to 60%. Finally it is concluded that by adjusting the conditions in co-spray drying process, the distribution amount and existence form of tanshinone II A in the outer layer of the particles can be changed so that to enhance lung inhaling performance of the drug composite particles.
Administration, Inhalation
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Desiccation
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Diterpenes, Abietane
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administration & dosage
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chemistry
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isolation & purification
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Drug Compounding
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methods
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Dry Powder Inhalers
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methods
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Microscopy, Electron, Scanning
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Microspheres
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Panax notoginseng
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chemistry
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Particle Size
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Plants, Medicinal
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chemistry
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Saponins
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administration & dosage
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chemistry
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isolation & purification
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Solubility
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X-Ray Diffraction
7.Preparation and characterization of tetrandrine-loaded PLGA nanocomposite particles by premix membrane emulsification coupled with spray-drying method.
Tao HU ; Hua-Xu ZHU ; Li-Wei GUO ; Lin-Mei PAN ; Bo LI ; Fei-Yan SHI ; Jin LU
Acta Pharmaceutica Sinica 2014;49(11):1607-1613
For effective inhalable dry-powder drug delivery, tetrandrine-PLGA (polylactic-co-glycolic acid) nanocomposite particles have been developed to overcome the disadvantages of nanoparticles and microparticles. The primary nanoparticles were prepared by using premix membrane emulsification method. To prepare second particles, they were spray dried. The final particles were characterized by scanning electron microscopy (SEM), dry laser particle size analysis, high performance liquid chromatography (HPLC), X-ray diffraction (XRD), differential scanning calorimetry (DSC), infrared analysis (IR) and confocal laser scanning microscope (CLSM). The average size of the primary particles was (337.5 ± 6.2) nm, while that second particles was (3.675 ± 0.16) μm which can be decomposed into primary nanoparticles in water. And the second particles were solid sphere-like with the drug dispersed as armorphous form in them. It is a reference for components delivery to lung in a new form.
Administration, Inhalation
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Benzylisoquinolines
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chemistry
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Calorimetry, Differential Scanning
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Drug Delivery Systems
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Dry Powder Inhalers
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Lactic Acid
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chemistry
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Microscopy, Electron, Scanning
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Nanocomposites
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chemistry
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Nanoparticles
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chemistry
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Particle Size
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Pharmaceutical Preparations
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Polyglycolic Acid
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chemistry
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X-Ray Diffraction