Comparação entre Reciproc Blue e quatro instrumentos réplicas: aspectos metalúrgicos, geometria, comportamento em torção e flexão / Comparison between Reciproc Blue and four replicalike instruments: metallurgical aspects, geometry, and behavior in torsion and flexion

A introdução da liga NiTi na endodontia proporcionou a fabricação de instrumentos com excelentes propriedades mecânicas, e uma das principais características é a possibilidade de alteração das temperaturas de transformação da liga, o qual pode possibilitar a presença de martensita em temperatura ambiente e consequentemente um efeito memória de forma. Entretanto, alguns dos sistemas comercializados atualmente possuem pouca ou nenhuma informação científica relatando suas propriedades mecânicas, características de design e métodos de fabricação. O objetivo deste trabalho foi comparar características geométricas, metalúrgicas e propriedades mecânicas (resistência à torção e flexão) de instrumentos Reciproc Blue (VDW, Munique, Alemanha), e quatro sistemas reciprocantes réplicas. Um total de 39 instrumentos de cada um dos sistemas reciprocantes, Reciproc Blue (RB), Prodesign R (PDR), V File (VF), V+ File (V+) e Univy One (UO) foram utilizados na pesquisa. O programa de Image J foi utilizado para mensuração dos diâmetros a cada milímetro da parte ativa e da área da seção transversal a 3 mm da ponta dos instrumentos. Imagens de MEV da parte ativa foram realizados para avaliar o acabamento superficial dos instrumentos. A composição atômica, fases presentes e temperaturas de transformação foram verificadas através de EDS, DRX e DSC, respectivamente. A flexibilidade foi aferida através de ensaios de dobramento até 45º conforme a especificação ISO 3630-1, e os ensaios de resistência à torção foram realizados de acordo com a especificação Nº28 ANSI/ADA. Todos os instrumentos apresentaram uma quantidade aproximadamente equiatômica de níquel e titânio. A análise qualitativa das fases cristalinas realizada através de ensaios de DRX, demonstrou a predominância de Fase R em todos os grupos, com exceção do grupo UO que apresenta uma mistura de fase R e martensita B19'. Na avaliação da área da seção, o instrumento RB obteve valores intermediários, os instrumentos PDR e V+ possuem menores valores e os instrumentos VF e UO possuem maiores valores. Observou-se grande impacto da geometria sobre as propriedades mecânicas, sendo que aqueles sistemas que apresentavam menor área que RB (PDR, V+) mostraram-se mais flexíveis e menos resistentes à torção (p<0.05), e o instrumento VF que teve maior área apresentou, como esperado, menos flexibilidade (p<0.05) e resistência torcional semelhante (p>0.05). A única exceção se deu com o sistema UO, que embora apresentasse uma maior área de seção, mostrou-se mais flexível e menos resistente à torção, provavelmente por influência da maior quantidade de martensita presente à temperatura ambiente. Nenhum dos instrumentos réplicas avaliados apresentaram características e comportamento mecânico iguais ao sistema padrão RB. Sugere-se que mais estudos devem ser realizados para a comparação do comportamento clínico destes instrumentos.

The introduction of NiTi alloy in endodontics has allowed the manufacturing of instruments with excellent mechanical properties, and one of the main characteristics is the ability to change alloy's transformation temperature, which can enable the presence of martensite at room temperature and consequently favor a shape memory effect. However, some of the currently marketed systems have limited or no scientific information regarding their mechanical properties, design characteristics, and manufacturing methods. The aim of this study was to compare the geometric characteristics, metallurgical aspects, and mechanical properties (torsional and flexural strength) of Reciproc Blue instruments (VDW, Munich, Germany) with four replica-like reciprocating systems. A total amount of 39 instruments from each reciprocating system, namely Reciproc Blue (RB), Prodesign R (PDR), V File (VF), V+ File (V+), and Univy One (UO), were used in the study. The Image J program was used to measure the diameters at every millimeter along the instruments active portion and the cross-sectional area at 3 mm from the instrument tip. SEM images of the active portion were obtained to evaluate the surface finishing of the instruments. Atomic composition, phases present, and transformation temperatures were determined through EDS, XRD, and DSC analyses, respectively. Flexibility was assessed by bending tests up to 45° according to ISO 3630-1 specifications, and torsional strength tests were performed according with ANSI/ADA Specification No. 28. All instruments exhibited an approximately equiatomic composition of nickel and titanium. Qualitative analysis of the crystalline phases using XRD tests demonstrated the predominance of the R-phase in all groups, except for the UO group, which exhibited a mixture of Rphase and B19' martensite. In terms of diameter and cross-sectional area evaluation, the RB instrument obtained intermediate values, while the PDR and V+ instruments had smaller values, and the VF and UO instruments had larger values. A significant impact of geometry on mechanical properties was observed, with systems exhibiting a smaller area than RB (PDR, V+) being more flexible and less torsion-resistant (p<0.05), and the VF instrument with a larger area showed, as expected, less flexibility (p<0.05) and similar torsional resistance (p>0.05). The only exception was the UO system, which, despite having a larger geometric configuration, exhibited greater flexibility and less torsional resistance, likely due to the higher amount of martensite present at room temperature. None of the replica-like instruments evaluated showed identical characteristics and mechanical behavior to the standard RB system. Further studies are suggested to compare the clinical performance of these instruments.

Evaluation of Physiochemical Properties, Thermal Behavior and Phytopharmaceutical Potential of Citrus aurantium’s Essential Oil

The study investigates the therapeutic potential of the Citrus aurantium var. amara essential oil extracted from the blossoms of the bitter orange plant by examining its chemical composition, thermal stability, and potency against infectious disease-causing pathogens. Initially, the volatile components of the essential oil were evaluated by obtaining a chromatographic fingerprint using HPTLC and FTIR spectrum identification. Furthermore, a thermal profile of the essential oil was obtained using the thermogravimetric-differential thermal analysis and differential scanning calorimetric analysis. A predetermined set of antibiotic-resistant microorganisms were used to examine the antibacterial activity of the essential oil. Lastly, its anti-inflammatory activity was assessed using the albumin denaturation assay. The research concluded that the Citrus aurantium var. Amara essential oil exhibits potential therapeutic characteristics which can be further explored through in vivo studies.

Preparação e caracterização de nanocarreadores de beta-lactose à base de pectina e lisozima / Preparation and characterization of beta-lactose nanocarriers based on pectin and lysozyme

O objetivo deste trabalho foi preparar e caracterizar nanocarreadores via auto-organização a partir da pectina de citros e lisozima para o encapsulamento da ß-lactose. Foram estudadas três condições de interação entre os biopolímeros variando a razão molar pectina/lisozima (3:1, 2:1, 1:1, 1:2 e 1:3), o pH e o tempo de aquecimento. A confirmação da interação foi determinada por espectroscopia no infravermelho por transformada de Fourier (FTIR) e por calorimetria de varredura diferencial (DSC). Os espectros de infravermelho evidenciaram que ligações de hidrogênio foram as principais forças envolvidas na formação dos nanocarreadores e sugeriram a ausência de ß-lactose livre na superfície das nanopartículas. Os termogramas evidenciaram que as nanopartículas formadas na presença de ß-lactose têm maior estabilidade térmica do que as nanopartículas sem ß-lactose. Para ambas as formulações estudadas, na presença e na ausência de ß-lactose, a formação das nanopartículas ocorreu entre os valores de pKa e ponto isoelétrico (pI) da pectina e lisozima, respectivamente, sendo a melhor razão de interação pectina/lisozima 1:2, em pH 10, a 80 ºC por 30 min. As nanopartículas foram formadas via auto-organização e todos as partículas apresentaram distribuição de tamanho homogênea, formato esférico, diâmetro inferior a 100 nm e carga superficial negativa. A morfologia e o tamanho das partículas pouco alteraram com a incorporação da -lactose. A eficiência de encapsulação (EE) da ß-lactose foi superior a 96% para as concentrações estudadas. Ensaios preliminares in vitro, em células epiteliais de câncer de cólon (HCT-116), evidenciaram que as nanopartículas formadas são capazes de adentrar no meio intracelular, possivelmente, por via endocitose

This work aimed to prepare and characterize nanocarriers via self-assembly using citrus pectin and lysozyme for ß-lactose encapsulation. Three interaction conditions between the biopolymers were studied, varying the pectin/lysozyme molar ratio (3:1, 2:1, 1:1, 1:2 and 1:3), pH and heating time. Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC) determined the interaction's confirmation. The infrared spectra showed that hydrogen bonds were the main forces involved in the formation of nanocarriers and suggested the absence of free ß-lactose on the surface of the nanoparticles. The thermograms showed that nanoparticles formed in the presence of ß-lactose have greater thermal stability than nanoparticles without ß-lactose. For both formulations studied, in the presence and absence of lactose, the formation of nanoparticles occurred between the pKa and isoelectric point (pI) values of pectin and lysozyme, respectively, with the best pectin/lysozyme interaction molar ratio 1:2, at pH 10, at 80 °C for 30 min. Nanoparticles were formed via self-assembly, and all particles presented homogeneous size distribution, spherical shape, diameter less than 100 nm, and negative surface charge. The morphology and size of the particles changed little with the incorporation of ß-lactose. The encapsulation efficiency (EE) of ß-lactose was higher than 96% for the concentrations studied. Preliminary in vitro assays in colon cancer epithelial cells (HCT-116) showed that the nanoparticles formed are capable of entering the intracellular medium, possibly via endocytosis

Analysis of Olibanum and Myrrha by Differential Scanning Calorimetry and Fourier Transform InfraRed / 国际中医中药杂志

Objective:To distinguish the differences between Olibanum and Myrrha by using modern analytical methods such as Differential Scanning Calorimeter (DSC) and Fourier Transform InfraRed (FT-IR). Methods:By collecting Olibanum and Myrrha in different growing areas and different processed prosecures, this paper to analizes the influence of temperature increase and its speed , as well as the particle size on the DSC experiment. The DSC method was used to perform a differential thermal map of Olibanum and Myrrha scanning and analysis; FT-IR was used to scan and analyze 20 batches of Olibanum and Myrrha. Results:TThe results of DSC analysis showed that the DSC experimental condition ranged between 30-600 ℃; the speed of temperature increase was 30 ℃/min; the particle size was 100 mesh. The DSC spectra of of Olibanum and Myrrha were significantly different. Only the processed products of frankincense had endothermic peak near 297 ℃, and there was no characteristic peak in this temperature range. Their exothermic peaks are close at 326 ℃, but their enthalpy values are quite different. The position of endothermic peak near 100 ℃ is close to the size of peak shape. FT-IR test showed that the absorption peaks of Olibanum and Myrrha at wave numbers 2 925, 1 710, 1 454, 1 371, 1 242, 1 029 cm -1 appeared, and the positions of strong peaks were also similar. The intensity of the characteristic peak of Myrrha wave number 1 029 cm -1 is greater than that of Olibanum. Conclusion:The DSC spectra of Olibanum and Myrrha are significantly different, and the difference between the two FT-IR spectra is small. Differential scanning Calorimetry is an effective, fast, and simple way to identify resinous Chinese medicinal materials, and is worthy of further popularization.

Caracterização mecânica, termodinâmica e química de fios CuNiTi ­ um estudo comparativo clínico e laboratorial / Mechanical, thermodynamic and chemical characterization of CuNiTi wires ­ a clinical and laboratory comparative study

Introdução: Os fios Copper Ni-Ti (CuNiTi) possuem indicações de uso clínico específicas, permanecendo no ambiente bucal por um longo período. Por esse motivo suas características mecânicas, termodinâmicas e estruturais devem ser preservadas durante todo o período de uso. Objetivos: Investigar se ocorrem alterações no comportamento mecânico, termodinâmico, estrutura e composição química superficial em fios CuNiTi 35°C submetidos ao envelhecimento in vivo (uso clínico) e in vitro (termociclagem), evidenciando as possíveis diferenças entre os métodos de envelhecimento. Material e Métodos: A amostra total foi constituída de 30 arcos pré-contornados 0.016", termodinâmicos com adição de cobre, e temperatura austenítica final (Af) de 35°C, da marca Ormco®. As análises destes fios resultaram em dois capítulos. Para o experimento clínico, 10 unidades de fios foram instaladas em 05 pacientes e permaneceram em meio bucal durante 30, 60 e 90 dias, e 05 fios foram analisados como recebidos (CR). A cada período, um hemiarco completo mais 1/3 (um terço) do hemiarco inferior direito foi retirado para análises. Para o experimento in vitro os 15 fios restantes foram submetidos à termociclagem para simulação do envelhecimento em ambiente oral durante 30 (600 ciclos), 60 (1200 ciclos) e 90 dias (1800 ciclos) com variação de temperatura entre 5°C e 55°C, com banhos de 90 segundos em cada temperatura, e transição de 15 segundos entre os banhos. Após cada período de envelhecimento in vivo e in vitro, os fios foram submetidos a um teste de padronização das suas dimensões através da medição dos diâmetros com paquímetro, Microscopia Eletrônica de Varredura (MEV), Espectrometria por Raios X Fluorescentes (FRX), ensaios de tração uniaxial e ensaio de Varredura Diferencial de Calorimetria (DSC). Resultados: No capítulo 1 a comparação entre os fios CR e os envelhecidos revelou que não houve diferença significativa entre os diâmetros das amostras, das forças obtidas ou mesmo das temperaturas Af, independentemente do tempo de permanência em boca. Foram encontrados predominantemente Ni, Ti, Cu e Al nas amostras, além de outros elementos químicos em concentrações variadas. No capítulo 2 não houve diferença significativa entre os diâmetros das amostras, das forças obtidas ou mesmo das temperaturas Af entre as amostras, independentemente do tempo ou do método de envelhecimento. Conclusão: As análises laboratoriais dos fios envelhecidos in vivo e in vitro foram comparadas, evidenciando que as características mecânicas, termodinâmicas e químicas dos fios permanecem estáveis mesmo até 90 dias de uso clínico ou 1800 ciclos de termociclagem. O método de envelhecimento in vitro se mostra uma alternativa viável para a análise destes parâmetros, em substituição aos métodos in vivo (AU).

Introduction: Copper Ni-Ti wires (CuNiTi) have specific indications for clinical use, remaining in the oral environment for a long period. For this reason, their mechanical, thermodynamic and structural characteristics must be preserved throughout the period of use of these materials. Objectives: To investigate whether there are changes in the mechanical, thermodynamic, structure and surface chemical composition of CuNiTi 35°C wires subjected to in vivo aging (clinical use) and in vitro (thermocycling), highlighting the possible differences between the aging methods. Material and Methods: The total sample was obtained from 30 pre-contoured Ormco® 0.016 thermodynamic archwires with copper addition and austenitic final temperature (Af) of 35°C. The analysis of these archwires resulted in two articles. For the clinical experiment, 10 units of wires were installed in 05 patients and remained in the oral environment for 30, 60 and 90 days, and 05 wires were analyzed as received. At each period, a complete hemiarch plus 1/3 of the right lower hemiarch was removed for analysis. For the in vitro experiment, the 15 remaining wires underwent thermocycling to simulate the aging of the oral environment for 30 (600 cycles), 60 (1200 cycles) and 90 days (1800 cycles) with a temperature range between 5°C and 55°C, with 90 second baths at each temperature, and 15 second transition between baths. After each in vivo and in vitro aging period, the wires underwent to a standardization test of their dimensions, by defining the diameters with a caliper, Scanning Electron Microscopy (SEM), Fluorescent X-Ray Spectrometry (FRX), tests of Uniaxial traction and Differential Scanning Calorimetry (DSC) test. Results: In chapter 1, the comparison between CR and aged wires revealed that there was no significant difference between the sample diameters, the forces obtained or even the temperatures Af, regardless the time spent in the mouth. Predominantly Ni, Ti, Cu and Al were found in the samples, in addition to other chemical elements in different concentrations. In chapter 2 there was no significant difference between the diameters of the samples, the forces obtained or even the temperatures Af between the samples, regardless of time or aging method. Conclusion: The comparison of the laboratoral analyzes of the archwires aged in vivo and in vitro showed that the mechanical, thermodynamic and the surface chemical characteristics were stable, even up to 90 days of clinical use or 1800 thermocycling cycles. The in vitro aging method is a viable alternative for the analysis of these parameters, replacing the in vivo methods (AU).

Pharmaceutical polymorphism of a 5´-O-oxalatoyl prodrug of zidovudine (azidothymidine)

The importance of polymorphism in pharmaceuticals makes its study relevant. The aim of this study was to investigatethe solid-state forms in which 3´-azido-2´, 3´-dideoxi-5´-O-oxalatoyl-thymidinic acid (AZT-Ac), a zidovudine (AZT)prodrug with improved pharmacokinetic properties, may exist. Samples were prepared using different crystallizationconditions and characterized using powder X-ray diffraction, solid-state nuclear magnetic resonance, differentialscanning calorimetry, thermogravimetry, and hot-stage microscopy. Pharmaceutical relevant properties such assolid-state stability and intrinsic dissolution rate (IDR) at 37°C in simulated gastric fluid (SGF) were also evaluated.AZT-Ac was found to able to exist as a crystalline polymorph (AZT-Ac-C) and an amorphous phase (AZT-Ac-A),which were thoroughly characterized. At 40°C/75% relative humidity (RH), AZT-Ac-A, in part, devitrified toAZT-Ac-C and partially hydrolyzed to AZT after 7 and 14 days of storage, respectively. AZT-Ac-C was physicallystable at 40°C/75% RH but partly hydrolyzed to AZT after 14 days of storage. In SGF, AZT-Ac-C exhibited a linearID profile and provided an ID rate of 0.494 mg/min/cm2, whereas AZT-Ac-A exhibited a nonlinear profile. Therefore,the crystalline form demonstrated the advantages over the amorphous one in terms of solid-state stability and IDR, butthe approaches to enhance its stability should be considered for further formulation of this prodrug.

Thermal analysis of some novel pyrimidine derivatives / Análisis térmico de algunos nuevos derivados de pirimidina

SUMMARY Some new pyrimidine derivatives have been synthesized and their decomposition characteristics have been studied by thermogravimetric and differential scanning calorimetric analysis. The thermal stability and some kinetics parameters of decomposition were evaluated from thermograms. It is observed that depending upon the structure, substitutions, thermal stability and decomposition kinetics varies in different compounds.

RESUMEN Se sintetizaron algunos nuevos derivados de pirimidina y se estudiaron sus características de descomposición mediante análisis termogravimétrico y calorimétrico diferencial de barrido. La estabilidad térmica y algunos parámetros cinéticos de descomposición se evaluaron a partir de los respectivos termogramas. Se observa que, dependiendo de la estructura y las sustituciones, la estabilidad térmica y la cinética de descomposición varían entre los diferentes compuestos.

Macromolecular properties and partial amino acid sequence of a Kunitz-type protease inhibitor from okra (Abelmoschus esculentus) seeds

A Kunitz-type protease inhibitor (OPI, okra protease inhibitor) has been purified from okra (Abelmoschus esculentus) seedsby a combination of ammonium sulfate precipitation, anion-exchange chromatography and reverse-phase high-performanceliquid chromatography. The protein shows an apparent mass of 21 kDa on sodium dodecyl sulfate-polyacrylamide gelelectrophoresis under reducing condition. OPI exhibits inhibitory activity against trypsin. Analysis of the far-UV circulardichroism spectrum showed that the protein contains *39% b-sheets but only *5% a-helices. The protein is thermallyquite stable, and exhibits a cooperative thermal unfolding transition at *70C, as determined by circular dichroismspectroscopy and differential scanning fluorimetry. De novo sequencing of OPI by nanoESI-Q-ToF mass spectrometry (MS)allowed the assignment of about 83% of its primary structure, which indicated that the protein shares 43% sequence identitywith a putative 21 kDa trypsin inhibitor from Theobroma bicolor. An intramolecular disulfide linkage between Cys149 andCys156 was also detected. The protein showed *24 and *25% sequence identity with a-amylase/subtilisin inhibitor frombarley and soybean (Kunitz) trypsin inhibitor, respectively. Comparative structure modeling of OPI revealed a structuralfold similar to other Kunitz-type TIs. The presence of Cys149–Cys156 disulfide bond as detected by MS and a seconddisulfide bond connecting Cys44–Cys91, conserved in all Kunitz-type TIs, is also identified in the model.

Study on thermophysical properties and effect of lyoprotectants in freezing human hepatoma Hep-G cells / 生物医学工程学杂志

Cell freeze-drying can be divided into the freezing and drying processes. Mechanical damage caused by ice crystals and damage from solute during freezing shall not be ignored and lyoprotectants are commonly used to reduce those damages on cells. In order to study the mechanism of lyoprotectants to protect cells and determine an optimal lyoprotectant formula, the thermophysical properties and percentage of unfrozen water of different lyoprotectants in freezing were investigated with differential scanning calorimeter (DSC). The survival rate indicated by trypan blue exclusion test and cell-attachment rate after 24 h using different lyoprotectants to freeze hepatoma Hep-G cells were measured after cell cryopreservation. The results show that 40% (W/V) PVP + 10% (V/V) glycerol + 15% (V/V) fetal bovine serum + 20% (W/V) trehalose formula of lyoprotectant demonstrate the best effect in protecting cells during freezing, for cell-attachment rate after 24 h is 44.56% ± 2.73%. In conclusion, the formula of lyoprotectant mentioned above can effectively protect cells.

Preparation and characterization of bioadhesive Bletilla striata polysaccharide and sodium alginate microspheres loaded with Panax notoginseng saponins / 中草药

Objective: Because of the adhesion of Bletilla striata polysaccharide (BSP), it was mixed with sodium alginate (SA) as a composite carrier to prepare mucoadhesive PNS-BSP composite microspheres. Panax notoginseng saponins (PNS) dispersion with sustained release property was used as an encapsulating drug. Methods: The composite microsphere was prepared by ion cross-linking method. The formulation process was investigated and optimized by single factor test and orthogonal design. The microspheres were evaluated by scanning electron microscope (SEM), particle size distribution, DSC, swelling properties, in vitro mucoadhesive properties, and in vitro release characteristics. Results: PNS-BSP composite microspheres had good roundness, rough surface and wrinkles. The microspheres showed a narrow size distribution. PNS was uniformly dispersed in microspheres in an amorphous state. The microspheres prepared by the best prescription process were stable in process and reproducible. Compared with the microspheres prepared by directly adding PNS, the drug loading, encapsulation efficiency and yield of PNS dispersion microspheres were increased significantly, which were 10.34%, 51.25%, and 82.21%, respectively. The drug loading, encapsulation efficiency, and yield were 4.04%, 12.16%, and 61.35% of PNS microspheres. The addition of BSP increased the swelling properties of the SA microspheres, and significantly increased the retention rate in the stomach of rats. The release of ginsenoside Rg1 in PNS-BSP microspheres was released slower compared to PNS. Conclusion: The bioadhesion of microspheres was increased by the addition of BSP. The drug loading, encapsulation efficiency, and yield of the microspheres were increased by the preparation of PNS as a dispersion, and the microspheres also had a certain sustained-release effect.

Advances on Characterization of Lyotropic Liquid Crystals as Drug Delivery System / 中国药学杂志

Lyotropic liquid crystal(LLC) is generally a kind of micelle association formed by self-assembly of amphiphilic lipid polymers in polar solvents. It have been applied in the study of drug delivery of administration of oral, skin injection, ocular, and cavity channel routes(including buccal cavity, nasal cavity, vagina), et al. Medical liquid crystal mainly includes lamellar phase, inverse hexagonal phase and inverse cubic phase. Inner assembling order in different structures of liquid crystals will affect the drug localization, viscosity, molecular interactions, and further drug release in vitro and in vivo, pharmacokinetics and so on. Thus, it is very important to characterize their microstructures. In this article, the characterization methods of LLC microstructures are comprehensively described based on the research of LLC as drug delivery carrier and related literatures, which can provide reference for further study of LLC drug delivery system.

Rapid identification of ginseng medicinal materials by differential scanning calorimetry / 国际中医中药杂志

Objective To explore a quick and simple method to identify ginseng medicinal materials. Methods Twenty types of ginseng medicinal materials were collected. The effects of two important factors:temperature and heating rate on differential scanning calorimetry (DSC) were investigated. The DSC features were used to quickly identify Radix et Rhizoma Notoginseng, Radix et Rhizoma Ginseng, Radix Panacis Quinquefolii and Panna ginseng C.A.Mey. Results The optimal experimental conditions for rapid identification of Radix et Rhizoma Notoginseng, Radix et Rhizoma Ginseng, Radix Panacis Quinquefolii and Panna ginseng C.A.Mey by DSC were determined: temperature range 30-400 ℃, heating rate 30 ℃/min. Under these conditions, the characteristic peak temperature and thermal enthalpy value can be used to distinguish four kinds of ginseng. Conclusions The experiment shows that the DSC method has the advantages of simple operation, rapid measurement, good reproducibility, easy analysis of the spectrum and less sample consumption. It is a new method for quickly identifying Chinese medicinal materials of ginseng genus.

Crystal form Analysis of Felodipine and Its Preparations / 中国药学杂志

OBJECTIVE: To clarify the crystal forms of the active pharmaceutical ingredient and preparations of felodipine from different sources, and explore the relationship between quality and efficacy of felodipine and its crystal form. METHODS: Crystal form characterization of the active pharmaceutical ingredient from different sources was carried out by powder X-ray diffraction (PXRD), infrared spectroscopy (IR) and differential scanning calorimetry (DSC). The Origin software was used to analyze the crystal forms of felodipine in the sample preparations from different sources. Biological evaluation in vivo was conducted by using whole animals. RESULTS: There were some differences in the crystal state of the active pharmaceutical ingredient from different sources, but the main components were basically the same, all of which were type I. Biological studies showed significant differences in the main pharmacokinetic parameters of felodipine sustained release tablets from different sources. Among them, the ρmax, tmax, t1/2, and AUC0-t had maximal 1.8, 1.4, 8.2 and 1.5 times of differences. CONCLUSION: Although the main crystal forms of felodipine bulk drug from different origins are consistent, the crystal state significantly changes after the preparation process. This finding is of important scientific significance to guide the improvement of process and product quality.

Cyclic fatigue resistance, torsional resistance, and metallurgical characteristics of M3 Rotary and M3 Pro Gold NiTi files

OBJECTIVES: To evaluate the mechanical properties and metallurgical characteristics of the M3 Rotary and M3 Pro Gold files (United Dental). MATERIALS AND METHODS: One hundred and sixty new M3 Rotary and M3 Pro Gold files (sizes 20/0.04 and 25/0.04) were used. Torque and angle of rotation at failure (n = 20) were measured according to ISO 3630-1. Cyclic fatigue resistance was tested by measuring the number of cycles to failure in an artificial stainless steel canal (60° angle of curvature and a 5-mm radius). The metallurgical characteristics were investigated by differential scanning calorimetry. Data were analyzed using analysis of variance and the Student-Newman-Keuls test. RESULTS: Comparing the same size of the 2 different instruments, cyclic fatigue resistance was significantly higher in the M3 Pro Gold files than in the M3 Rotary files (p < 0.001). No significant difference was observed between the files in the maximum torque load, while a significantly higher angular rotation to fracture was observed for M3 Pro Gold (p < 0.05). In the DSC analysis, the M3 Pro Gold files showed one prominent peak on the heating curve and 2 prominent peaks on the cooling curve. In contrast, the M3 Rotary files showed 1 small peak on the heating curve and 1 small peak on the cooling curve. CONCLUSIONS: The M3 Pro Gold files showed greater flexibility and angular rotation than the M3 Rotary files, without decrement of their torque resistance. The superior flexibility of M3 Pro Gold files can be attributed to their martensite phase.

Preparation and in vitro/in vivo evaluation of polydatin solid dispersion / 中草药

Objective: Polydatin solid dispersion (PD-SD) was prepared for improving bioavailability. Methods: In this study, PD-SD was prepared by solvent evaporation method with dissolution as index for improving bioavailability. The physicochemical properties of PD-SD were evaluated by Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), X-ray power diffraction (XRD), and scanning electron microscope (SEM). HPLC was employed to determine the plasma concentration of PD-SD with PD crude drug as reference group in rats after oral administration. Results: FT-IR revealed that there was no new chemical bond between drug and carrier. DSC and XRD results indicated that PD in PD-SD was amorphous. SEM results showed that the morphology of PD-SD was close to irregular globular. The AUCs of PD-SD and PD were 328.79 and 139.70 μg·min/mL after oral administration, respectively. Conclusion: PD-SD is prepared by simple technology. PD-SD significantly improved the in vitro dissolution and oral bioavailability of PD in rats.

Effect of essential oil from asarum on percutaneous delivery of sinapine and its mechanism / 中草药

Objective: To study the enhancing effect of essential oil from asarum (EOA) on percutaneous delivery of sinapine and its mechanism. Methods: Transepidermal water loss (TEWL) was determined with Vapo Meter to evaluate the decrease of skin barrier by asarum essential oil. In vitro permeation of sinapine through rat skin was performed in the presence or absence of EOA, and the permeated cumulative amount and retention of sinapine were compared. In vivo percutaneous test was further performed to estimate the improvement of EOA on percutaneous delivery of sinapine. Attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and differential scanning calorimeter (DSC) were used to evaluate the changes of lipid and protein in stratum corneum. Results: TEWL value increased after the treatment of EOA, which indicated the decrease of skin barrier. The permeated cumulative amount and retention of sinapine in the presence of EOA were higher than those in the absence of EOA, and in vivo percutaneous test further confirmed this issue. After EOA treatment, the lipid and protein disorder could be observed from ATR-FTIR and DSC map, which indicated the increasing of skin permeability. Conclusion: EOA can enhance the percutaneous delivery of sinapine through improving the disorder of lipid and protein of stratum corneum.

Preparation of PEGylated graphene oxide nanoparticles loaded with oridonin and its inhibitory effects on human colon cancer / 中草药

Objective To prepare PEGylated graphene oxide nanoparticles (GO-PEG-NPs) loaded with oridonin (ORI) and investigate its inhibitory effect on human colon cancer. Methods 4-armed PEG was grafted onto GO via an amidation process and GO-PEG was characterized by IR and TGA. Then, ORI, a widely used cancer chemotherapy drug, was absorbed onto GO-PEG via blending. The encapsulation efficiency and drug loading ratio were measured by UV. The cytotoxicity of ORI-GO-PEG, GO-PEG, and free ORI on SW620 and HT29 human colon cancer cells were evaluated using MTT assay. In vivo anti-tumor activity of ORI-GO-PEG-NPs were evaluated in mice bearing SW620 tumor. Results IR and TGA data indicated that 4-armed PEG was successfully coupled with GO and UV data showed that the encapsulation efficiency and drug loading ratio were 95.81% and 48.92%, respectively. Moreover, ORI-GO-PEG-NPs showed good stability in physiological condition. The results of cytotoxicity test indicated that compared to free ORI, the ORI-GO-PEG-NPs exhibited higher cytotoxicity in SW620 and HT29 cells. Meanwhile, it was confirmed that ORI-GO-PEG- NPs could significantly inhibit the growth of SW620 tumor in vivo compared with ORI. Conclusion The obtained ORI-GO-PEG-NPs displayed excellent drug-loading capacity and better tumor inhibitory effect. These results provided the experimental basis for development of anticancer drug delivery system.

Preparation of fisetin solid dispersions / 中成药

AIM To prepare fisetin solid dispersions.METHODS Melting method and solvent method were used for the preparation of solid dispersions,respectively.With carrier type,drug-carrier ratio and stirring time as influencing factors,accumulative dissolution rate as an evaluation index,the preparation was optimized by orthogonal test on the basis of single factor experiment.The interaction between drug and carrier was investigated by Fourier transform infrared spectroscopy (FTIR),and the drug existing state was analyzed by differential scanning calorimetry (DSC).RESULTS Solvent method was more suitable for the preparation of solid dispersions.The optimal conditions were determined to be PVPK-30 as a carrier,1 ∶ 12 for drug-carrier ratio,and 30 min for stirring time,the accumulative dissolution rate reached 90.87％ within 20 min.There might be a hydrogen bond association between PVPK-30 and fisetin previously existing in amorphous or molecular state.CONCLUSION The dissolution rate of fisetin can be obviously increased after being prepared into solid dispersions.

Silver nanoparticle incorporation effect on mechanical and thermal properties of denture base acrylic resins

ABSTRACT Objective The aim of the present study was to evaluate the mechanical and thermal characteristics of two denture base acrylic resins containing silver nanoparticles (AgNPs). Material and Methods Two different acrylic denture base resins (heat-polymerized and microwave polymerized) containing 0.3, 0.8 and 1.6 wt% AgNPs were evaluated for flexural strength, elastic modulus and impact strength. The glass transition temperature (Tg) and relative heat capacity (Cp) of the samples were determined from the Differential Scanning Calorimetry (DSC) results. For statistical analysis, two-way ANOVA and Tukey-HSD tests were performed. Results Addition of 0.8% and 1.6% AgNPs in microwave-polymerized resin significantly decreased the transverse strength and elastic modulus. In terms of impact strength, the addition of AgNPs has no effect on both resin groups. Glass transition temperature (Tg) was decreased with the addition of AgNPs for both denture base resins. Conclusions The incorporation of AgNPs, generally used for antimicrobial efficiency, affected the transverse strength of the denture base acrylic resins depending on the concentration of nanoparticles. Tg was decreased with the addition of AgNPs for both denture base resins.

Importancia clínica del punto austenítico final en la selección de las aleaciones de níquel-titanio para su aplicación en arcos utilizados en Ortodoncia / Clinical importance of austenitic final point in the selection of nickel-titanium alloys for application in orthodontic-use arches

Resumen: Existe en el mercado una gran cantidad de alambres de aleaciones de níquel-titanio; sin embargo, no todos poseen las características ideales de memoria de forma y superelasticidad para ser utilizados en ortodoncia. El objetivo de este estudio fue encontrar la temperatura austenitica final de estos arcos con la finalidad de determinar la fase de transformación para su mejor uso clínico en Ortodoncia. Métodos: Se estudiaron once alambres de níquel-titanio más utilizados en Ortodoncia y se evaluó la fase de transformación utilizando la prueba de calorimetría de barrido diferencial. Conclusiones: Este estudio muestra cómo algunos arcos de NiTi en Ortodoncia presentan resultados contrarios a los que promocionan.

Abstract: There are many nickel-titanium alloy wires available in the market. Nevertheless not all of them possess the ideal characteristics of shape memory and super-elasticity to be used in orthodontic treatment. The aim of the present study was to find austenitic final temperature of these archwires so as to determine the transformation phase in order to better use them in orthodontics. Methods: Eleven nickel-titanium orthodontic wires were selected. Transformation phase was assessed using differential scanning calorimetry method. Conclusions: The present study illustrates how some orthodontic Ni-Ti wires elicit results contrary to those advertised.