Guided by the concept of quality by design(QbD), this study optimizes the calcination and quenching process of calcined Magnetitum and establishes the XRD characteristic spectra of calcined Magnetitum, providing a scientific basis for the formulation of quality standards. Based on the processing methods and quality requirements of Magnetitum in the Chinese Pharmacopoeia, the critical process parameters(CPPs) identified were calcination temperature, calcination time, particle size, laying thickness, and the number of vinegar quenching cycles. The critical quality attributes(CQAs) included Fe mass fraction, Fe~(2+) dissolution, and surface color. The weight coefficients were determined by combining Analytic Hierarchy Process(AHP) and the criteria importance though intercrieria correlation(CRITIC) method, and the calcination process was optimized using orthogonal experimentation. Surface color was selected as a CQA, and based on the principle of color value, the surface color of calcined Magnetitum was objectively quantified. The vinegar quenching process was then optimized to determine the best processing conditions. X-ray diffraction(XRD) was used to establish the characteristic spectra of calcined Magnetitum, and methods such as similarity evaluation, cluster analysis, and orthogonal partial least squares-discriminant analysis(OPLS-DA) were used to evaluate the quality of the spectra. The optimized calcined Magnetitum preparation process was found to be calcination at 750 ℃ for 1 h, with a laying thickness of 4 cm, a particle size of 0.4-0.8 cm, and one vinegar quenching cycle(Magnetitum-vinegar ratio 10∶3), which was stable and feasible. The XRD characteristic spectra analysis method, featuring 9 common peaks as fingerprint information, was established. The average correlation coefficient ranged from 0.839 5-0.988 1, and the average angle cosine ranged from 0.914 4 to 0.995 6, indicating good similarity. Cluster analysis results showed that Magnetitum and calcined Magnetitum could be grouped together, with similar compositions. OPLS-DA discriminant analysis identified three key characteristic peaks, with Fe_2O_3 being the distinguishing component between the two. The final optimized processing method is stable and feasible, and the XRD characteristic spectra of calcined Magnetitum was initially established, providing a reference for subsequent quality control and the formulation of quality standards for calcined Magnetitum.
X-Ray Diffraction/methods* ; Drugs, Chinese Herbal/chemistry* ; Quality Control ; Particle Size

The present study explored the effect of co-amorphous technology in improving the dissolution rate and stability of silybin based on the puerarin-silybin co-amorphous system prepared by the spray-drying method. Solid-state characterization was carried out by powder X-ray diffraction(PXRD), polarizing microscopy(PLM), Fourier transform infrared spectroscopy(FT-IR), differential scanning calorimetry(DSC), etc. Saturated powder dissolution, intrinsic dissolution rate, moisture absorption, and stability were further investigated. The results showed that puerarin and silybin formed a co-amorphous system at a single glass transition temperature which was higher than that of any crude drug. The intrinsic dissolution rate and supersaturated powder dissolution of silybin in the co-amorphous system were higher than those of the crude drug and amorphous system. The co-amorphous system kept stable for as long as three months under the condition of 40 ℃, 75% relative humidity, which was longer than that of the single amorphous silybin. Therefore, the co-amorphous technology could significantly improve the dissolution and stability of silybin.
Calorimetry, Differential Scanning ; Desiccation ; Drug Compounding/methods* ; Drug Stability ; Silybin ; Solubility ; Spectroscopy, Fourier Transform Infrared ; Technology ; X-Ray Diffraction

There has been increasing use of the H₂O₂-based teeth bleaching agents. The purpose of this study was to evaluate the bleaching effectiveness of the laser irradiation combined with nitrogen doped-TiO₂ nanoparticles (NPs) on the stained resin. Nitrogen (N) doped-TiO₂ NPs were prepared under sol-gel method. Light absorbance, X-ray diffraction patterns of NPs, and bleaching of methylene blue and stained resins were evaluated. For bleaching of stained resin, NPs-containing gel was used. For irradiation, light of two different wavelengths was used. Unlike TiO₂, N-TiO₂ showed high absorbance after 400 nm. N-TiO₂, which have used TiN as a precursor, showed a new rutile phase at the TiN structure. For methylene blue solution, N-TiO₂ with 3% H₂O₂ resulted in the greatest absorbance decrease after laser irradiation regardless of wavelength. For stained resin test, N-TiO₂ with 3% H₂O₂ resulted in the greatest color difference after laser irradiation, followed by group that used N-TiO₂ without 3% H₂O₂.
Methods ; Methylene Blue ; Nanoparticles ; Nitrogen ; Tin ; Tooth Bleaching Agents ; X-Ray Diffraction

PURPOSE: The purpose of this study was to investigate the corrosion behaviors of dental implant alloy after micro-sized surface modification in electrolytes containing Mn ion. MATERIALS AND METHODS: Mn-TiO₂ coatings were prepared on the Ti-6Al-4V alloy for dental implants using a plasma electrolytic oxidation (PEO) method carried out in electrolytes containing different concentrations of Mn, namely, 0%, 5%, and 20%. Potentiodynamic method was employed to examine the corrosion behaviors, and the alternating-current (AC) impedance behaviors were examined in 0.9% NaCl solution at 36.5℃±1.0℃ using a potentiostat and an electrochemical impedance spectroscope. The potentiodynamic test was performed with a scanning rate of 1.667 mV s⁻¹ from −1,500 to 2,000 mV. A frequency range of 10⁻¹ to 10⁵ Hz was used for the electrochemical impedance spectroscopy (EIS) measurements. The amplitude of the AC signal was 10 mV, and 5 points per decade were used. The morphology and structure of the samples were examined using field-emission scanning electron microscopy and thin-film X-ray diffraction. The elemental analysis was performed using energy-dispersive X-ray spectroscopy. RESULT: The PEO-treated surface exhibited an irregular pore shape, and the pore size and number of the pores increased with an increase in the Mn concentration. For the PEO-treated surface, a higher corrosion current density (I(corr)) and a lower corrosion potential (E(corr)) was obtained as compared to that of the bulk surface. However, the current density in the passive regions (I(pass)) was found to be more stable for the PEO-treated surface than that of the bulk surface. As the Mn concentration increased, the capacitance values of the outer porous layer and the barrier layer decreased, and the polarization resistance of the barrier layers increased. In the case of the Mn/Ca-P coatings, the corroded surface was found to be covered with corrosion products. CONCLUSION: It is confirmed that corrosion resistance and polarization resistance of PEO-treated alloy increased as Mn content increased, and PEO-treated surface showed lower current density in the passive region.
Alloys ; Corrosion ; Dental Implants ; Dielectric Spectroscopy ; Electric Impedance ; Electrolytes ; Manganese ; Methods ; Microscopy, Electron, Scanning ; Plasma ; Spectrum Analysis ; X-Ray Diffraction

PURPOSE: The purpose of this study was to compare the optical properties of pre-colored dental monolithic zirconia ceramics of various thicknesses sintered in a microwave and those in a conventional furnace. MATERIALS AND METHODS: A2-shade of pre-colored monolithic zirconia ceramic specimens (22.0 mm × 22.0 mm) in 3 thickness groups of 0.5, 1.0, and 1.5 mm were divided into 2 subgroups according to the sintering methods (n=9): microwave and conventional sintering. A spectrophotometer was used to obtain CIELab color coordinates, and translucency parameters and CIEDE2000 color differences (ΔE 00) were measured. The relative amount of monoclinic phase (X(m)) was estimated with x-ray diffraction. The surface topography was analyzed by atomic force microscope and scanning electron microscope. Statistical analyses were conducted with two-way ANOVA (α=.05). RESULTS: There were small interaction effects on CIE L*, a*, and TP between sintering method and thickness (P<.001): L* (partial eta squared η(p)²=0.115), a* (η(p)²=0.136), and TP (η(p)²=0.206), although higher b* values were noted for microwave sintering regardless of thickness. Color differences between two sintering methods ranged from 0.52 to 0.96 ΔE(00) units. The X(m) values ranged from 7.03% to 9.89% for conventional sintering, and from 7.31% to 9.17% for microwave sintering. The microwave-sintered specimen demonstrated a smoother surface and a more uniform grain structure compared to the conventionally-sintered specimen. CONCLUSION: With reduced processing time, microwave-sintered pre-colored dental monolithic zirconia ceramics can exhibit similar color perception and translucency to those by conventional sintering.
Ceramics* ; Clothing ; Color Perception ; Methods ; Microwaves* ; Spectrophotometry ; X-Ray Diffraction

PURPOSE: The physicochemical properties of a xenograft are very important because they strongly influence the bone regeneration capabilities of the graft material. Even though porcine xenografts have many advantages, only a few porcine xenografts are commercially available, and most of their physicochemical characteristics have yet to be reported. Thus, in this work we aimed to investigate the physicochemical characteristics of a porcine bone grafting material and compare them with those of 2 commercially available bovine xenografts to assess the potential of xenogenic porcine bone graft materials for dental applications. METHODS: We used various characterization techniques, such as scanning electron microscopy, the Brunauer-Emmett-Teller adsorption method, atomic force microscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, and others, to compare the physicochemical properties of xenografts of different origins. RESULTS: The porcine bone grafting material had relatively high porosity (78.4%) and a large average specific surface area (SSA; 69.9 m²/g), with high surface roughness (10-point average roughness, 4.47 µm) and sub-100-nm hydroxyapatite crystals on the surface. Moreover, this material presented a significant fraction of sub-100-nm pores, with negligible amounts of residual organic substances. Apart from some minor differences, the overall characteristics of the porcine bone grafting material were very similar to those of one of the bovine bone grafting material. However, many of these morphostructural properties were significantly different from the other bovine bone grafting material, which exhibited relatively smooth surface morphology with a porosity of 62.0% and an average SSA of 0.5 m²/g. CONCLUSIONS: Considering that both bovine bone grafting materials have been successfully used in oral surgery applications in the last few decades, this work shows that the porcine-derived grafting material possesses most of the key physiochemical characteristics required for its application as a highly efficient xenograft material for bone replacement.
Adsorption ; Bioprosthesis ; Bone Regeneration ; Bone Transplantation ; Chemical Phenomena ; Dental Materials ; Durapatite ; Heterografts* ; Methods ; Microscopy, Atomic Force ; Microscopy, Electron, Scanning ; Porosity ; Spectrum Analysis ; Surgery, Oral ; Transplants* ; X-Ray Diffraction

OBJECTIVEThis study investigated the effects of hydroxyapatite (HA)/chitosan (CS)-transforming growth factor-β1 (TGF-β1) composite coatings on titanium surfaces, as well as on the attachment and proliferation of osteoblasts.

METHODSHA/CS-TGF-β1 composite coatings were prepared on titanium surfaces by physical, chemical, and biological modifications. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FTIR), and other methods were employed to analyze the chemical composition and surface topography of the composite coatings. CCK-8 and immunofluorescence assays were used to analyze the effects of the coatings on the attachment and proliferation of osteoblasts.

RESULTSHA/CS-TGF-β1 composite coatings were successfully prepared. Their contact angle was almost zero. These composite coatings were applied in vitro, with a drug released early and a burst release effect. The growth of osteoblasts was not inhibited on it and it had obvious promoting effect on the adhesion and early proliferation of osteoblasts.

CONCLUSIONThe composite coatings significantly promote the adhesion and early proliferation of osteoblasts in vitro. This finding shows that the proposed method demonstrates a good prospective application in surface modification of titanium.

Cell Proliferation ; Chitosan ; chemistry ; Dental Bonding ; methods ; Durapatite ; chemistry ; Microscopy, Electron, Scanning ; Osteoblasts ; physiology ; Prospective Studies ; Spectroscopy, Fourier Transform Infrared ; Surface Properties ; Titanium ; chemistry ; Transforming Growth Factor beta ; chemistry ; Transforming Growth Factors ; X-Ray Diffraction

OBJECTIVE: Different methods have been utilized to prevent enamel demineralization and other complications during orthodontic treatment. However, none of these methods can offer long-lasting and effective prevention of orthodontic complications or interventions after complications occur. Considering the photocatalytic effect of TiO2 on organic compounds, we hoped to synthesize a novel bracket with a TiO2 thin film to develop a photocatalytic antimicrobial effect. METHODS: The sol-gel dip coating method was used to prepare TiO2 thin films on ceramic bracket surfaces. Twenty groups of samples were composed according to the experimental parameters. Crystalline structure and surface morphology were characterized by X-ray diffraction and scanning electron microscopy, respectively; film thickness was examined with a surface ellipsometer. The photocatalytic properties under ultraviolet (UV) light irradiation were analyzed by evaluating the degradation ratio of methylene blue (MB) at a certain time. Antibacterial activities of selected thin films were also tested against Lactobacillus acidophilus and Candida albicans. RESULTS: Films with 5 coating layers annealed at 700℃ showed the greatest photocatalytic activity in terms of MB decomposition under UV light irradiation. TiO2 thin films with 5 coating layers annealed at 700℃ exhibited the greatest antimicrobial activity under UV-A light irradiation. CONCLUSIONS: These results provide promising guidance in prevention of demineralization by increasing antimicrobial activities of film coated brackets.
Candida albicans ; Ceramics* ; Crystallins ; Dental Enamel ; Esthetics ; Hope ; Lactobacillus acidophilus ; Methods ; Methylene Blue ; Microscopy, Electron, Scanning ; Ultraviolet Rays ; X-Ray Diffraction

Deformities in tissues and organs can be treated by using tissue engineering approach offering the development of biologically functionalized scaffolds from a variety of polymer blends which mimic the extracellular matrix and allow adjusting the material properties to meet the defect architecture. In recent years, research interest has been shown towards the development of chitosan (CS) based biomaterials for tissue engineering applications, because of its minimal foreign body reactions, intrinsic antibacterial property, biocompatibility, biodegradability and ability to be molded into various geometries and forms thereby making it suitable for cell ingrowth and conduction. The present work involves the fabrication of nanofibrous scaffold from CS and poly(vinyl alcohol) blends by free-surface electrospinning method. The morphology and functional characteristics of the developed scaffolds were assessed by field emission scanning electron microscopy and fourier transformed infra-red spectra analysis. The morphological analysis showed the average fiber diameter was 269 nm and thickness of the mat was 200–300 µm. X-ray diffraction study confirmed the crystalline nature of the prepared scaffolds, whereas hydrophilic characteristic of the prepared scaffolds was confirmed by measured contact angle. The scaffolds possess an adequate biodegradable, swelling and mechanical property that is found desirable for tissue engineering applications. The cell study using umbilical cord blood-derived mesenchymal stem cells has confirmed the in vitro biocompatibility and cell supportive property of the scaffold thereby depicting their potentiality for future clinical applications.
Biocompatible Materials ; Chitosan ; Congenital Abnormalities ; Crystallins ; Extracellular Matrix ; Foreign Bodies ; Fourier Analysis ; Fungi ; In Vitro Techniques ; Mesenchymal Stromal Cells ; Methods ; Microscopy, Electron, Scanning ; Nanofibers* ; Polymers ; Tissue Engineering* ; Umbilical Cord ; X-Ray Diffraction

Herpetospermum caudigerum lignans (HTL), one of the potential drugs with anti-hepatitis B virus and hepatoprotective effects, has limited clinical applications because of poor aqueous solubility and low bioavailability. Both herpetrione (HPE) and herpetin (HPN) are the most abundant ingredients in HTL and exhibit weak acidity. The purpose of the present study was to produce dried preparations of HTL (composed of HPE and HPN) nanosuspensions (HTL-NS) with high redispersibility using lyophilization technology. The HTL-NS was prepared by utilizing precipitation-combined homogenization technology based on acid-base neutralization reactions, and critical formulation and process parameters affecting the characteristics of HTL-NS were optimized. The resultant products were characterized by particle size analysis, SEM, XRD, stability, solubility, dissolution and in vivo bioavailability. HTL-NS showed near-spherical-shaped morphology and the size was 243 nm with a narrow PDI value of 0.187. The dried preparations with a relatively large particle size of 286 nm and a PDI of 0.215 were achieved by using 4% (W/V) mannitol as cryoprotectants, and had a better stability at 4 or 25 °C for 2 months, compared to HTL-NS. In the in vitro test, the dried preparations showed markedly increased solubility and dissolution velocity. Besides, in the in vivo evaluation, it exhibited significant increases in AUC, CMRT and a decrease in T, compared to the raw drug. In conclusion, our results provide a basis for the development of a drug delivery system for poorly water-soluble ingredients with pH-dependent solubility.
Animals ; Biological Availability ; Cell Line ; Chemistry, Pharmaceutical ; methods ; Drug Carriers ; chemistry ; Drug Delivery Systems ; Humans ; Lignans ; administration & dosage ; chemistry ; pharmacokinetics ; Male ; Nanoparticles ; administration & dosage ; chemistry ; Particle Size ; Rats ; Rats, Wistar ; Solubility ; X-Ray Diffraction