Haematitum and Limonitum are two iron-containing mineral medicines included in the 2020 edition of the Chinese Pharmacopoeia. They have similar main components and major differences in their property, flavor, channel tropism, and clinical uses. In this study, we investigated the surface properties, mineral composition, mineral dissociation, elemental composition, and iron state of Haematitum and Limonitum to explore their mineralogical differences. Scanning electron microscopy(SEM), specific surface and porosity analyzer, X-ray diffractometer(XRD), X-ray photoelectron spectrometer(XPS), and advanced mineral identification and characterization system(AMICS) were used to analyze the mineralogy of Haematitum and Limonitum. The results showed that Haematitum had an angular surface with granular attachments and a specific surface area of 17.04 m~2·g~(-1). In comparison, Limonitum had a smooth and flat surface with a bundled acicular crystal structure and a specific surface area of 46.29 m~2·g~(-1). Haematitum consists of 31 detectable minerals containing 18 elements, with the major element, iron(44.5% Fe~(2+) and 55.5% Fe~(3+)) distributed in 17 minerals, including hematite, iron oxide, knebelite, siderite, and magnesioferrite. Limonitum consists of 32 detectable minerals containing 17 elements, with the major element, iron(14.5% Fe~(2+) and 85.5% Fe~(3+)) distributed in 19 minerals, including limonite, iron oxide, chlorite, and knebelite. In summary, the elemental composition of Haematitum and Limonitum does not differ greatly, but there are large differences in the mineral composition and iron state. The large specific surface area and strong adsorption capacity of Limonitum may be one of the mechanisms of its anti-diarrheal action. The Fe_2O_3 and illite contained in Haematitum and Limonitum may be the key substances for their hemostasis effects. The mineralogical differences are expected to provide a reference for explaining the scientific connotation of mineral medicine and laying a material foundation for studying its mechanism of action.
Iron/analysis* ; Minerals/chemistry* ; Drugs, Chinese Herbal/chemistry* ; X-Ray Diffraction ; Microscopy, Electron, Scanning ; Photoelectron Spectroscopy

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

To optimize the traditional refining process of Hydrargyrum Chloratum Compositum(HCC) and explore the change law of substances before and after refining, this study applied the hierarchical analysis method(AHP)-entropy weight method, using appearance, yield, and mercuric chloride content as evaluation indexes. The temperature and time of mild and strong fire were examined as single factors, and an L_9(3~4) orthogonal experiment was used to optimize the refining process. An infrared thermal imaging platform was set up to record the temperature changes on the surface of the tank, aiming to establish a standardized operating procedure for the refining process. Elemental changes, physical phase changes, and thermal property changes of the materials before and after refining were analyzed using atomic absorption spectrophotometry(AAS), X-ray diffraction(XRD) and differential scanning calorimetry(DSC). The results showed that the average overall score of the finished product obtained from the optimized HCC refining process(with mild fire temperature of 102 ℃, mild fire refining time of 30 min, strong fire temperature of 178 ℃, and strong fire refining time of 68 min) was 91.59, with an RSD of 0.076%, indicating that the process is stable and feasible. Combined with thermal imaging data and related research results, it was found that, at the strong fire temperature, mercury ions and nitrate ions generated mercuric chloride under the catalysis of other ions. The mercury content of mercurous chloride, mercuric chloride synthesized from nitric acid, HCC, and the pre-refined sample was 84.535%, 72.376%, 70.838%, and 41.334%, respectively. The highest intensity of the(120) diffraction peak for HCC appeared around 20.36°, but the residual fit value was larger. The synthesis of mercuric chloride from HCC and nitric acid showed an exothermic peak at 190-204 ℃, with the peak shape exhibiting a rightward trend. This study optimized the traditional refining process of HCC and analyzed the elemental changes, physical phase changes, and thermal property changes before and after refining. The findings provide experimental data for exploring the changing patterns in the refining process of HCC and its pharmacological value, as well as for standardizing the traditional refining process in clinical practice.
Drugs, Chinese Herbal/chemistry* ; X-Ray Diffraction ; Temperature ; Calorimetry, Differential Scanning ; Mercuric Chloride/chemistry*

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

PURPOSE: The aim of this study was to investigate the effect of different numbers of heat treatments applied to superstructure porcelain on optical, thermal, and phase formation properties of zirconia.MATERIALS AND METHODS: Forty zirconia specimens were prepared in the form of rectangular prism. Specimens were divided into four groups (n = 10) according to the number of firing at heating values of porcelain. Color differences and translucency parameter were measured, and X-ray diffraction (XRD) analysis and differential scanning calorimetry (DSC) were performed. Data were analyzed with analysis of variance (ANOVA).RESULTS: There were no statistically significant differences in ΔE, TP, L, a, and b value changes of the zirconia specimens as a result of repetitive firing processes (P>.05).CONCLUSION: Although additional firing processes up to 4 increase peak density in thermal analysis, additional firing processes up to 4 times can be applied safely as they do not result in a change in color and phase character of zircon frameworks.
Calorimetry, Differential Scanning ; Dental Porcelain ; Fires ; Heating ; Hot Temperature ; X-Ray Diffraction

PURPOSE: The purpose of this study was to evaluate the effects of various protocols and systems for finishing and polishing monolithic zirconia on surface topography, phase transformation, and bacterial adhesion. MATERIALS AND METHODS: Three hundred monolithic zirconia specimens were fabricated and then treated with three finishing and polishing systems (Jota [JO], Meisinger [ME], and Edenta [ED]) using four surface treatment protocols: coarse finishing alone (C); coarse finishing and medium polishing (CM); coarse finishing and fine polishing (CF); and coarse finishing, medium polishing, and fine polishing (CMF). Surface roughness, crystal phase transformation, and bacterial adhesion were evaluated using atomic force microscopy, X-ray diffraction, and streptococcal biofilm formation assay, respectively. One-way and two-way analysis of variance with Tukey post hoc tests were used to analyze the results (α=.05). RESULTS: In this study, the surface treatment protocols and systems had significant effects on the resulting roughness. The CMF protocol produced the lowest roughness values, followed by CM and CF. Use of the JO system produced the lowest roughness values and the smallest biofilm mass, while the ME system produced the smallest partial transformation ratio. The ED group exhibited the highest roughness values, biofilm mass, and partial transformation ratio. CONCLUSION: Stepwise surface treatment of monolithic zirconia, combined with careful polishing system selection, is essential to obtaining optimal microstructural and biological surface results.
Bacterial Adhesion ; Biofilms ; Clinical Protocols ; Dental Polishing ; Microscopy, Atomic Force ; X-Ray Diffraction

PURPOSE: To evaluate the influence of cyclic loading on phase transformation of zirconia abutments and to compare the effectiveness of three different quantitative ageing assessment techniques. MATERIALS AND METHODS: Thirty two Y-TZP prostheses fabricated from two brands, InCoris ZI and Ceramill ZI, were cemented to titanium bases and equally divided into two subgroups (n=8): control group without any treatment and aged group with cyclic loading between 20 N and 98 N for 100,000 cycles at 4 Hz in distilled water at 37℃. The tetragonal-to-monoclinic phase transformation was assessed by (i) conventional x-ray diffraction (XRD), (ii) micro x-ray diffraction (µXRD), and (iii) micro-Raman spectroscopy. The monoclinic-phase fractions (M%) were compared by two-way ANOVA. RESULTS: InCoris Zi presented significantly higher M% than Ceramill Zi in both control and aged groups (P<.001). Both materials exhibited significant phase transformation with monoclinicphase of 1 to 3% more in aged groups than controls for all thre e assessment techniques. The comparable M% was quantified by both µXRD and XRD. The highest M% was assessed with micro-Raman. CONCLUSION: Cyclic loading produced significant phase transformation in tested Y-TZP prostheses. The micro-Raman spectroscopy could be used as an alternative to XRD and µXRD.
Prostheses and Implants ; Spectrum Analysis ; Titanium ; Water ; X-Ray Diffraction

The single-factor test was used to optimize the high-pressure homogenization method to prepare the phenolic extract nanosuspensions(DBNs). The physicochemical properties of the obtained nanosuspensions were characterized and the cumulative release in vitro was evaluated. The results showed that the drug concentration was 0.5 g·L~(-1), the mass concentrations of PVPK30 and SDS were 0.5 and 0.25 g·L~(-1), respectively, the probe ultrasonic time was 5 min, the homogenization pressure was 900 bar, and the number of homogenization was 2 times. The prepared DBNs had an average particle size of(168.80±0.36) nm, polydispersity index(PDI) of 0.09±0.04, stability index(SI) of 0.85, and DBNs were stable for storage within 30 days. Scanning electron microscopy showed that the particle size of the dragon's blood extract was reduced and the uniformity was improved in the obtained nanosuspensions. X-ray diffraction pattern and differential scanning calorimetry showed that the phenolic extract of dragon's blood was still in an amorphous state after being prepared into nanosuspensions. The results of saturated solubility measurement showed that the solubility of DBNs lyophilized powder reached 6.25 g·L~(-1), while the solubility of DB raw powder was only 28.67 mg·L~(-1). The in vitro dissolution experiments showed that DBNs lyophilized powder accumulated in gastrointestinal fluid for 8 h. The release amount was 90%,the cumulative release of the raw powder in the gastrointestinal fluid for 24 h was less than 1%, and the solubility and dissolution rate of the DBNs lyophilized powder were significantly higher than the DB raw powder. The method is simple in process and convenient in operation, and can successfully prepare uniform and stable nanosuspensions to improve its solubility, and provides a research basis for solving the application limitation of dragon's blood extract.
Calorimetry, Differential Scanning ; Nanoparticles ; Particle Size ; Plant Extracts ; chemistry ; Solubility ; Suspensions ; X-Ray Diffraction

The powder X-ray diffraction(PXRD) technique was used to investigate fourteen kinds of Ranunculaceae herbal decoction pieces(RHDP) recorded in Chinese Pharmacopoeia and to explore a novel PXRD quality control method for RHDP. The results indicated that only three RHDP-Paeoniae Radix Alba, Paeoniae Radix Rubra, and Moutan Cortex, contained calcium oxalate monodydrate(COM), whereas no COM existed in other eleven kinds of RHDP. The difference in PXRD for Paeoniae Radix Alba and Paeoniae Radix Rubra from different growing areas were investigated. The quantitative analysis method for COM was discussed by considering the water-boiling manufacturing process of herbal decoction pieces. The water-boiling experiments revealed that the PXRD peaks from COM crystals in RHDP were enhanced significantly after boiling. Paeoniae Radix Alba, Paeoniae Radix Rubra, Moutan Cortex, Aconiti Lateralis Radix Praeparata, Aconiti Radix, Aconiti Kusnezoffii Radix, and Anemone Raddeanae Rhizoma exhibited a similar series of broader peaks in the 2θ region of 15° to 35°, whose origins were discussed on the basis of chemical constituents RHDP reported by other researchers. These diffraction broader peaks most likely originated from periodic orientation of benzene ring in organic molecular crystals of aconitine-and paeonolum-based alkaloids and glycosides chemical constituents, subsequently, possibly from some other organic constituents. The PXRD technique can be used to rapidly identify Cimicifuga heracleifolia with an amorphous dispersion peak and C. dahurica with a sharp-peak feature. Climatidis Radix et Rhizoma exhibited a series of sharp PXRD peaks. The PXRD method can provide a valuable quality control method for RHDP.
Aconitum ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Paeonia ; chemistry ; Phytochemicals ; analysis ; Ranunculaceae ; chemistry ; Rhizome ; chemistry ; X-Ray Diffraction

BACKGROUND: Nowadays, production of nanocomposite scaffolds based on natural biopolymer, bioceramic, and metal ions is a growing field of research due to the potential for bone tissue engineering applications. METHODS: In this study, a nanocomposite scaffold for bone tissue engineering was successfully prepared using collagen (COL), beta-tricalcium phosphate (β-TCP) and strontium oxide (SrO). A composition of β-TCP (4.9 g) was prepared by doping with SrO (0.05 g). Biocompatible porous nanocomposite scaffolds were prepared by freeze-drying in different formulations [COL, COL/β-TCP (1:2 w/w), and COL/β-TCP-Sr (1:2 w/w)] to be used as a provisional matrix or scaffold for bone tissue engineering. The nanoparticles were characterized by X-ray diffraction, Fourier transforms infrared spectroscopy and energy dispersive spectroscopy. Moreover, the prepared scaffolds were characterized by physicochemical properties, such as porosity, swelling ratio, biodegradation, mechanical properties, and biomineralization. RESULTS: All the scaffolds had a microporous structure with high porosity (~ 95–99%) and appropriate pore size (100–200 µm). COL/β-TCP-Sr scaffolds had the compressive modulus (213.44 ± 0.47 kPa) higher than that of COL/β-TCP (33.14 ± 1.77 kPa). In vitro cytocompatibility, cell attachment and alkaline phosphatase (ALP) activity studies performed using rat bone marrow mesenchymal stem cells. Addition of β-TCP-Sr to collagen scaffolds increased ALP activity by 1.33–1.79 and 2.92–4.57 folds after 7 and 14 days of culture, respectively. CONCLUSION: In summary, it was found that the incorporation of Sr into the collagen-β-TCP scaffolds has a great potential for bone tissue engineering applications.
Alkaline Phosphatase ; Animals ; Biopolymers ; Bone and Bones ; Bone Marrow ; Collagen ; Fourier Analysis ; Freeze Drying ; In Vitro Techniques ; Ions ; Mesenchymal Stromal Cells ; Nanocomposites ; Nanoparticles ; Porosity ; Rats ; Spectrum Analysis ; Strontium ; X-Ray Diffraction