Calendula officinalis L. flower extract-mediated green synthesis of silver nanoparticles under LED light

Abstract Silver nanoparticles (AgNPs) are among the most known nanomaterials being used for several purposes, including medical applications. In this study, Calendula officinalis L. flower extract and silver nitrate were used for green synthesis of silver nanoparticles under red, green and blue light-emitting diodes. AgNPs were characterized by Ultraviolet-Visible Spectrophotometry, Field Emission Scanning Electron Microscopy, Dynamic Light Scattering, Electrophoretic Mobility, Fourier Transform Infrared Spectroscopy and X-ray Diffraction. Isotropic and anisotropic silver nanoparticles were obtained, presenting hydrodinamic diameters ranging 90 - 180 nm, polydispersity (PdI > 0.2) and moderate stability (zeta potential values around - 20 mV)

Potential Alendronate Sodium drug carrier by preparation and characterization of sodium alginate cross-linked Montmorillonite

Abstract In drug therapy, it is important to provide therapeutic levels of drug to the site of action and maintain them during the treatment. This work describes the in vitro release of alendronate from sodium alginate cross-linked Montmorillonite (MMT) composite beads. Effect of crosslinking cation, concentration of montmorillonite and media on encapsulation efficiencies, and release profiles of alendronate were studied. Beads were characterized using equilibrium swelling ability study, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Energy-dispersive x-ray spectroscopy (EDX) and scanning electron microscopy (SEM). Results indicate that addition of montmorillonite increases the encapsulation efficiencies and slows down the release rates significantly.

Ganoderma applanatum extract mediated synthesis of silver nanoparticles

Abstract Nanotechnology has been used in the field of medicine and pharmacology for its greater efficacy of drug delivery than crude molecules of drugs. In the present study medicinal mushroom Ganoderma applanatum extract mediated silver nanoparticles (AgNPs) were synthesized, characterized by Ultraviolet-visible (UV-Vis.) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction, Dynamic light scattering (DLS) and Furior transform-infrared (FTIR) spectroscopy. Maximum absorbance was recorded at 435nm by UV-Vis. The synthesized nanoparticles of 13.54nm-255nm in size with an average particle size of 58.77nm were analyzed by DLS. FTIR-Spectroscopy provided high transmission at 3606cm-1 corresponds for phenolic capping biochemical. Thus G. applanatum extract can be used for synthesis of silver nanoparticles and the synthesized nanoparticles may be used for development of future therapeutic agent for treatment of diseases.

Cristalogénesis biológica y cristalografía en la elucidación de la estructura tridimensional de las proteínas. Revisión narrativa / Protein tridimensional structure by biological crystallogenesis and crystallography. Narrative review

La obtención de información estructural tridimensional de una proteína es de suma importancia en campos tan variados como la bioquímica funcional, las ciencias de materiales o biomédicas. Siendo actualmente la difracción de rayos X de monocristal el estándar de oro para la consecución de este objetivo, la obtención de dicho monocristal sigue siendo un cuello de botella desde el punto de vista práctico, y poco entendido desde el punto de vista teórico. En este artículo se revisa desde la perspectiva estructural de la proteína la forma en que los rayos X permiten obtener la información estructural y las condiciones fisicoquímicas que permiten la formación de un cristal adecuado para estos experimentos.

Obtaining three-dimensional structural information of a protein is of utmost importance in various fields such as functional biochemistry, materials science, or biomedical sciences. Even though single crystal X-ray diffraction is currently the gold standard for this purpose, growing said single crystal is still a bottleneck from a practical viewpoint, and not fully understood from a theoretical point of view. In this article, we review, from a protein structure perspective, the way X-rays provide structural information, and the physicochemical conditions that promote the formation of an adequate crystal for these experiments.

Influence of alumina air-abrasion for highly translucent partially stabilized zirconia on flexural strength, surface properties, and bond strength of resin cement

Abstract Objective This study aims to evaluate the influence of different air-abrasion pressures and subsequent heat treatment on the flexural strength, surface roughness, and crystallographic phases of highly translucent partially stabilized zirconia (Y-PSZ), and on the tensile bond strength of resin cement to Y-PSZ. Methodology Fully sintered zirconia specimens were ground with SiC paper (control) and/or air-abraded with 50 µm particles of alumina at 0.1, 0.15, 0.2, or 0.3 MPa or left as-sintered. After air-abrasion at 0.2 MPa (0.2AB), additional specimens were then heated to 1500°C, and held for one hour at this temperature (0.2AB+HT1h). Flexural strength and surface roughness were evaluated. Crystalline phase identification was also carried out using X-ray diffraction. Bonded zirconia specimens with self-adhesive resin cement were stored in distilled water at 37°C for 24 h, either with or without aging (thermal cycling 4-60°C/20000). Results were analyzed statistically by ANOVA and Tukey-Kramer tests. Results The flexural strength decreased with the increase in air-abrasion pressure, while in contrast, the surface roughness increased. The lowest flexural strength and the highest roughness value were found for the 0.2AB and 0.3AB groups, respectively. All groups contained cubic-, tetragonal ( t )-, and rhombohedral ( r )-ZrO2 phases with the exception of the as-sintered group. Upon increasing the air-abrasion pressure, the relative amount of the r -ZrO2 phase increased, with a significant amount of r -ZrO2 phase being detected for the 0.2AB and 0.3AB groups. The 0.2AB+HT1h group exhibited a similar flexural strength and t -ZrO2 phase content as the as-sintered group. However, the 0.2AB group showed a significantly higher tensile bond strength (p<0.05) than the 0.2AB+HT1h group before and after aging. Conclusion Micromechanical retention by alumina air-abrasion at 0.2 MPa, in combination with chemical bonding of a resin to highly translucent Y-PSZ using a MDP-containing resin cement may enable durable bonding.

The effect of silver nanoparticles on composite shear bond strength to dentin with different adhesion protocols

Abstract In Dentistry, restorative materials and oral bacteria are believed to be responsible for restoration failure. To make long-lasting restorations, antibacterial agents should be made. Inorganic nanoparticles and their nano composites are applied as good antibacterial agents. Objective The purpose of this study was to investigate the effect of silver nanoparticles on composite shear bond strength using one etch and rinse and one self-etch adhesive systems. Material and Methods Silver nanoparticles were prepared. Transmission electron microscope and X-ray diffraction were used to characterize the structure of the particles. Nanoparticles were applied on exposed dentin and then different adhesives and composites were applied. All samples were tested by universal testing machine and shear bond strength was assesed. Results Particles with average diameter of about 20 nm and spherical shape were found. Moreover, it was shown that pretreatment by silver nanoparticles enhanced shear bond strength in both etch and rinse, and in self-etch adhesive systems (p≤0.05). Conclusions Considering the positive antibacterial effects of silver nanoparticles, using them is recommended in restorative dentistry. It seems that silver nanoparticles could have positive effects on bond strength of both etch-and-rinse and self-etch adhesive systems. The best results of silver nanoparticles have been achieved with Adper Single Bond and before acid etching.

Solubility and dissolution studies of tibolone polymorphs

ABSTRACT Different solid forms of an active pharmaceutical ingredient can have distinct chemical and physical characteristics. In this work, we studied the solubility and dissolution properties of the described tibolone polymorphic forms (I and II). Both forms were successively recrystallized and characterized by powder X-ray diffraction and attenuated total reflection infrared spectroscopy. Equilibrium solubility and dissolution profiles were performed for both forms. Solubility studies demonstrated that form II is statistically more soluble in water, 0.01 mol L-1 HCl and pH 4.5 acetate buffer. The solubility of forms I and II were explained in terms of crystal packing. Dissolution tests of tablets showed a lower release of polymorphic form II than form I from tablets. The results showed an impact of polymorphism on the quality of tibolone tablets and suggest that tibolone forms I and II can show distinct interactions with pharmaceutical excipients used in tablets. Therefore, only form I is acceptable for the preparation of tablet forms. Based on our results, we propose the quality control on tibolone raw materials using X-ray diffraction analysis and attenuated total reflection infrared spectroscopy.

Corrosion behavior of zirconia in acidulated phosphate fluoride

ABSTRACT Objective The corrosion behavior of zirconia in acidulated phosphate fluoride (APF) representing acidic environments and fluoride treatments was studied. Material and Methods Zirconia rods were immersed in 1.23% and 0.123% APF solutions and maintained at 37°C for determined periods of time. Surfaces of all specimens were imaged using digital microscopy and scanning electron microscopy (SEM). Sample mass and dimensions were measured for mass loss determination. Samples were characterized by powder X-ray diffraction (XRD) to detect changes in crystallinity. A biosensor based on electrochemical impedance spectroscopy (EIS) was used to detect ion dissolution of material into the immersion media. Results Digital microscopy revealed diminishing luster of the materials and SEM showed increased superficial corrosion of zirconia submerged in 1.23% APF. Although no structural change was found, the absorption of salts (sodium phosphate) onto the surface of the materials bathed in 0.123% APF was significant. EIS indicated a greater change of impedance for the immersion solutions with increasing bathing time. Conclusion Immersion of zirconia in APF solutions showed deterioration limited to the surface, not extending to the bulk of the material. Inferences on zirconia performance in acidic oral environment can be elucidated from the study.

The use of the software JST-XRD for identification of crystalline phases in pharmaceutical raw materials and tablets / Uso do software JST-XRD para identifcação de fases cristalinas em insumos farmacêuticos e medicamentos

Study of polymorphism is of great importance for the pharmaceutical industry once polymorphs may display different physicochemical properties, which, in turn, may result in stability differences that can bring problems for the manufacturing stages and the quality of fnal products. Although research on organic polymorphs has greatly increased in the last decades, it still does not cover all needs for the pharmaceutical market. Techniques such as spectroscopy in the infrared region, nuclear magnetic resonance, thermal analysis, X-ray diffraction, etc., can be used to identify polymorphism. The polymorphism is a property of the crystalline solid state, and can be evaluated by X-ray diffraction once each polymorph exhibits one specifc X-ray diffraction pattern. The JST-XRD program is a tool designed to help the identifcation of crystalline phases (including polymorphs) present in pharmaceutical ingredients and tablets by using X-ray diffraction data obtained from scientifc articles and patents. This paper presents new implementations for the JST-XRD and describes its use in the analysis of active pharmaceutical ingredient and marketed tablets of norfloxacin, mebendazole and atorvastatin calcium. By the means of comparison, JSTXRD allowed identifying the crystalline phases in the diffraction patterns of the analyzed drugs, showing the program suitability for polymorphism research, pre-formulation and quality control in pharmaceutical industries. JST-XRD can also be used for educational purposes in undergraduate and graduate programs in order to show the potentiality of X-ray powder diffraction in polymorphism analysis.(AU)

O estudo do polimorfsmo é de grande importância na indústria farmacêutica porque os polimorfos podem apresentar diferentes propriedades físico-químicas, podendo resultar em diferenças na estabilidade e desse modo causar problemas nas etapas de manufatura e no produto fnal. Embora a pesquisa de moléculas orgânicas que apresentam polimorfsmo tenha aumentado bastante nas últimas décadas, ainda não contempla todas as necessidades do mercado farmacêutico. Para a identifcação de polimorfsmo podem ser utilizadas técnicas como espectroscopia na região do infravermelho, ressonância nuclear magnética, análise térmica (DSC), difração de raios X, etc. O polimorfsmo, por ser uma propriedade do estado sólido e cristalino, pode ser avaliado através da difração de raios X, já que cada polimorfo apresenta um padrão de difração de raios X único. O programa JST-XRD é uma ferramenta projetada para auxiliar a identifcação de fases cristalinas, incluindo polimorfos, presentes em insumos farmacêuticos e comprimidos, usando dados de difração de raios X obtidos em artigos científcos e patentes. Esse trabalho apresenta novas implementações no JST-XRD e descreve seu uso na análise de amostras de princípio ativo e comprimidos comerciais de norfloxacino, mebendazol e atorvastatina cálcica. Através das comparações realizadas, JSTXRD permitiu identifcar todas as fases cristalinas dos difratogramas dos fármacos analisados, mostrando que o programa é adequado para pesquisa em polimorfsmo; na pré-formulação e controle de qualidade em indústrias farmacêuticas, assim como para uso didático em cursos de graduação e pós-graduação a fm de mostrar as potencialidades da difração de raios X na análise de polimorfsmo.(AU)

Obtenção de gel mucoadesivo de nistatina para o tratamento da candidíase oral. Desenvolvimento e caracterização de dispersões sólidas de nistatina / Mucoadhesive gel obtaining nystatin for the treatment of oral candidiasis. Development and characterization of solid dispersions of nystatin

A nistatina (NYS) é o fármaco de primeira escolha no tratamento da candidíase oral, que frequentemente acomete mais os indivíduos imunocomprometidos e pacientes com outras desordens (diabetes não tratada, neoplasias, imunodeficiências). No mercado brasileiro, a NYS é encontrada na forma de suspensão oral aquosa, onde o procedimento para sua administração consiste em bochechar o medicamento. Apesar de haver a indicação de que se mantenha o contato direto entre fármaco e a mucosa oral, na qual se encontra a Candida spp., o que aumentaria expressivamente o sucesso terapêutico, a suspensão não apresenta tal propriedade. Assim, a NYS que é fármaco com ação efetiva contra a candidíase oral, é considerada pertencente à Classe IV do Sistema de Classificação Biofarmacêutica, ou seja, apresenta baixa solubilidade e baixa permeabilidade. A baixa solubilidade pode comprometer sua disponibilidade na cavidade oral, e consequentemente, sua ação farmacológica. Diante desse quadro, o objetivo do presente trabalho foi o desenvolvimento de dispersões sólidas de NYS para o tratamento da candidíase oral, e sua posterior incorporação em gel mucoadesivo oral, favorecendo a formulação no local de ação. As dispersões sólidas são sistemas farmacêuticos, onde um fármaco pouco solúvel em água encontra-se dispersado em um carreador, no estado sólido. Os carreadores normalmente são hidrofílicos, o que permite que esses sistemas sejam empregados para aumentar a solubilidade aquosa do fármaco. Assim, foram desenvolvidas as dispersões sólidas de NYS, pelo método de eliminação do solvente, empregando como carreadores, lactose, HPMC, poloxamer 407 e poloxamer 188. Essas foram submetidas à caracterização por análise térmica, usando os ensaios de calorimetria exploratória diferencial (DSC) e termogravimetria/termogravimetria derivada (TG/DTG). Dentre essas dispersões sólidas, aquelas que se mostraram com comportamento térmico sugerindo a formação de um novo "sistema", foram analisadas por meio de ensaio de solubilidade. Dessa forma, a formulação NYS DS G2 (49) se destacou, pois apresentou maior solubilidade em água (4,484 mg/mL); em pH 5,5 (4,249 mg/mL) e em pH 7,0 (4,293 mg/mL), ou seja, houve um aumento de 1,426 vezes em água; 4,227 vezes em pH 5,5; e 2,743 vezes em pH 7,0. Essa formulação foi, por fim avaliada por difração de raio-X e espectroscopia de infravermelho com transformada de Fourier, técnicas que corroboraram com a análise térmica quanto à indicação de formação da dispersão sólida. Por sua vez, essa dispersão sólida foi incorporada em 4 bases de géis mucoadesivos de carbopol ® 934 PNF, alterando apenas a concentração do polímero (0,5; 1,0; 1,5; 2,0 %p/p). Foi observado que a liberação de NYS DS G2 (49) foi superior, quando comparada à liberação de NYS MP a partir do gel, e através do ensaio de mucoadesão, percebeu-se que os géis desenvolvidos apresentaram propriedades mucoadesivas compatíveis com relatos na literatura, independentemente da quantidade de carbopol ® empregada. As características reológicas foram distintas, e foi observado que as formulações Gel A e Gel B, que possuem menor quantidade de polímero, tiverem um indicativo de comportamento de fluido newtoniano, diferente dos demais, o que pode não ser desejado para esse tipo de forma farmacêutica tópica e semi-sólida. Ao final desse trabalho, pode-se concluir que foi possível desenvolver um sistema farmacêutico na forma de dispersão sólida com maior solubilidade que a NYS pura, e sua incorporação em uma forma farmacêutica mucoadesiva, e que a liberação da NYS na forma DS foi muito superior que o fármaco na forma "convencional", o que permite que a NYS esteja mais disponível na cavidade oral, e também junto à mucosa bucal, o que levaria a efeito farmacológico mais efetivo do antifúngico

Nystatin (NYS) is the drug of first choice in the treatment of oral candidiasis that most often affect immunocompromised individuals, and patients with other disorders. In the Brazilian market, NYS is found in the form of aqueous oral suspension, a medication used in the form of mouthwash. Although there is an indication to maintain direct contact between the drug and the oral mucosa, where Candida spp. is found, as well as where therapeutic success would significantly be increased, the suspension has no such property. Thus, the NYS is an effective drug against oral candidiasis, and belongs to Class IV of the Biopharmaceutical Classification System, it has low solubility and low permeability. The low solubility can compromise its availability in the oral cavity, and consequently, its pharmacological action. Given this situation, the objective of this work was the development of solid dispersions of NYS for the treatment of oral candidiasis, and its subsequent incorporation into oral mucoadhesive gel, in order to facilitate its action. Solid dispersions are pharmaceutical systems, in which a solid drug poorly soluble in water is dispersed in a carrier. These carriers are usually hydrophilic, and this allows the systems to be employed in order to increase the aqueous solubility of the drug. Thus, the solid NYS dispersions were developed by the solvent evaporation method, employing lactose, HPMC, poloxamer 407 and poloxamer 188 as carrier. These samples were subjected to characterization by thermal analysis, using differential scanning calorimetry (DSC) and thermogravimetry / derivative thermogravimetry (TG / DTG). Among these solid dispersions, those samples which showed a specific thermal behavior suggesting the formation of new "system" were analyzed by solubility test. Thus, the NYS DS G2 formulation (49) stood out, once it showed greater solubility in water (4.484 mg/mL); at pH 5.5 (4.249 mg/mL) and pH 7.0 (4.293 mg/mL), in other words, an increase of 1,426 times in water; 4,227 times at pH 5.5; and 2,743 times at pH 7.0. This formulation was finally evaluated by X-ray diffraction, infrared spectroscopy with Fourier transform, techniques that corroborate the thermal analysis, indicating the formation of the solid dispersion. On the other hand, this solid dispersion was incorporated into 4 Carbopol ® 934 PNF mucoadhesive gels, with a variation of the polymer concentration. It was observed that NYS is improved of delivery from the gels, employing mucoadhesion test, and was also observed that the gels have mucoadhesive properties consistent with reports in the literature. However, the rheological characteristics are different, and it was observed that the Gel A and Gel B formulations, which has a lower amount of polymer behaved as a Newtonian fluid, which may not be desired for this type of topical gel. As conclusion, it was possible to develop a pharmaceutical system in the form of solid dispersion with greater solubility than the pure NYS, and their incorporation in a mucoadhesive dosage form and the release of NYS as DS was far superior wherein the drug in the "conventional" manner, which allows the NYS is longer available in the oral cavity, and also adjacent to the buccal mucosa, leading to more effective pharmacological effect of the antifungal agent

Early onset intellectual disability in chromosome 22q11.2 deletion syndrome / Inicio temprano de discapacidad intelectual en el Síndrome de deleción del cromosoma 22q11.2

Chromosome 22q11.2 deletion syndrome, or DiGeorge syndrome, or velocardiofacial syndrome, is one of the most common multiple anomaly syndromes in humans. This syndrome is commonly caused by a microdelection from chromosome 22 at band q11.2. Although this genetic disorder may reflect several clinical abnormalities and different degrees of organ commitment, the clinical features that have driven the greatest amount of attention are behavioral and developmental features, because individuals with 22q11.2 deletion syndrome have a 30-fold risk of developing schizophrenia. There are differing opinions about the cognitive development, and commonly a cognitive decline rather than an early onset intellectual disability has been observed. We report a case of 22q11.2 deletion syndrome with both early assessment of mild intellectual disabilities and tetralogy of Fallot as the only physic manifestation.

El síndrome del cromosoma 22q11.2, también conocido como supresión o síndrome de DiGeorge o síndrome velocardiofacial, es uno de los síndromes más comunes de anomalías múltiples en los seres humanos. Este síndrome es comúnmente causado por una microdeleción del cromosoma 22 en q11.2 banda. Aunque este trastorno genético muestra varias anomalías clínicas y diferentes grados de compromiso orgánico, las características clínicas que han atraído la mayor atención son el comportamiento y el desarrollo, porque las personas con síndrome de deleción 22q11.2 tienen un riesgo 30 veces mayor de desarrollar esquizofrenia. Hay diferentes opiniones sobre el desarrollo cognitivo, y comúnmente se se ha observado un deterioro cognitivo en lugar de un inicio temprano de discapacidad intelectual. Presentamos un caso de síndrome de deleción 22q11.2 tanto con la evaluación temprana de discapacidades intelectuales leves como con la tetralogía de Fallot como única manifestación física.

Identificación de dos formas polimórficas cristalinas de clopidogrel bisulfato en materia prima farmacéutica / Identification of two polymorphic forms of clopidogrel bisulphate crystal in pharmaceutical raw materials

Introducción: el clopidogrel bisulfato existe en numerosas formas cristalinas, que varían en su estabilidad fisicoquímica, por lo que algunas de estas formas, patentadas o no, son útiles en la fabricación de medicamentos. Objetivo: identificar las formas cristalinas existentes en dos muestras de clopidogrel bisulfato materia prima comercializadas para la fabricación de medicamentos y el estado de pureza de ambas muestras. Métodos: las muestras de materia prima se obtuvieron de una industria nacional. Se examinaron mediante técnicas analíticas avanzadas como difracción de rayos X, calorimetría diferencial de barrido, termogravimetría y espectroscopia infrarroja. Se compararon los valores encontrados con los del estado del arte reconocidos en la literatura revisada para el clopidogrel bisulfato materias primas y tomados como referencia. Resultados: se obtuvieron los difractogramas, termogramas y espectros de absorción correspondientes a las muestras analizadas. Se utilizó el software TA Universal Analysis para obtener el porcentaje de descomposición, punto de fusión y picos identificadores en las muestras. Conclusiones: la muestra 1 contiene la forma cristalina I del bisulfato de clopidogrel, que no es pura ya que existe una banda característica de la presencia de contaminación con la forma cristalina II. La muestra 2 corresponde a la forma cristalina II del producto en forma pura(AU)

Introduction: clopidogrel bisulphate exists in many crystalline forms that vary in their physicochemical stability: some of these forms either patented or not are useful in the drug production. Objective: to identify the existing crystalline forms in two samples of Clopidogrel bisufhate raw material for the drug and the purity index of both samples. Methods: the raw material samples were taken from a domestic industry. They were tested through advanced analytical techniques such as differential scanning calorimetry, X-ray scattering pattern, infrared spectroscopy and thermogravimetric analysis. The final values were then compared with the well-established state-of-the-art values found in the reviewed literature for the clopidrogrel bisulfate raw materials and accepted as reference. Results: the physicochemical parameters were obtained from the absorption spectra, thermograms and diffractograms. The TA Universal Analysis software yielded the percentage of decomposition, the melting points and the peak identifiers in the samples. Conclusions: its was concluded that the sample 1 contained the crystal form I of the Clopridogrel bisulfate that is not a pure one since there is a characteristic band indicating contamination with the crystalline form II. The sample 2 had the pure crystalline form II of the product(AU)

Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

Synthesis and Crystal Structure of Two Nitro-Regioisomers of cis-4(4-Methoxyphenyl)-3-Methyl-2-Phenyl-1, 2, 3, 4-Tetrahydroquinoline / Síntesis y estudio de la estructura cristalina de dos nitro regioisómerosde la cis-4-(4-metoxifenil)-3-metil-2-fenil-1, 2, 3, 4-tetrahydroquinolina

Dos nitro-regioisómeros de la moléculacis-4-(4-metoxifenil)-3-metil-2-fenil-1,2,3,4-tetrahydroquinolina fueronpreparados vía una síntesis one-pot de tres componentes basada en lareacción de cicloadición imino Diels-Alder catalizada por BF3.OEt2. Sucompleta caracterización estructural se llevó a cabo usando la técnicade difracción de rayos-X de monocristal y métodos espectroscópicos.La pureza de los productos y la composición de las mezclas de reacciónfueron monitoreadas por cromatografía en capa fina (CCD). Losproductos fueron aislados y purificados usando cromatografía encolumna. Las sustancias fueron identificadas usando resonancia magnéticanuclear (RMN) y espectrometría de masas (EM). Los datos para lacaracterización por difracción de rayos-X fueron colectados usando undifractómetro Bruker AFC7S Mercury con radiación de Mo-Kα (λ =0.71073Å) a temperatura ambiente. Las estructuras de los regio-isómerosfueron confirmadas por 1H RMN y 13C RMN y la estructura cristalinafue estudiada usando la difracción de rayos-X de monocristal. El análisisespectroscópico (RMN, EM y difracción de rayos-X) mostró una completacaracterización y permitió establecer la correcta estereoquímica para elanillo tetrahidroquinolínico. El empaquetamiento molecular en el cristalpara el regioisómero 5-nitro 4 es producto de la combinación de enlaces dehidrógeno intermoleculares e interacciones de van der Waals, mientras queen el 7-nitro regioisómero 3 el empaquetamiento se debe principalmente ainteracciones intermoleculares débiles de tipo van der Waals y N—H••• π...

Here we synthesized two nitro regioisomersof cis-4-(4-methoxyphenyl)-3-methyl-2-phenyl-1,2,3,4-tetrahydroquinoline via the “one pot” three-componentimino Diels-Alder reaction catalyzed by BF3.OEt2and completed its structural characterization using thesingle crystal X-ray diffraction technique and otherspectroscopic methods. To monitor the purity of theproducts and the composition of the reaction mixtureswe used thin layer chromatography, and isolated andpurified the products by column chromatography. Thenusing nuclear magnetic resonance (NMR) and massspectrometry (MS) identified the substances. We collectedX-ray diffraction data for crystal characterization byusing a Bruker AFC7S Mercury diffractometer with Mo-Kα radiation (λ = 0.71073Å) at room temperature. Thestructures of these regioisomers were confirmed by 1HNMR and 13C NMR studies and studied their crystalstructure using single crystal X-ray diffraction technique.The spectroscopy analyses (NMR, GC-MS and X-raydiffraction) provided a complete characterizationand enabled the correct stereochemistry for thetetrahydroquinoline ring. We determined the molecularpacking for the 5-nitro regioisomer 4 is the product ofthe combination of intermolecular hydrogen bonds andvan der Waals interactions, while for 7-nitro regioisomer3 is mainly due to weak intermolecular van der Waalsinteractions and N—H··· π...

Dois nitro regioisómeros da molécula cis-4-(4-metoxifenil)-3-metil-2-fenil-1,2,3,4-tetrahydroquinolina foram preparados através de umasíntese de um só recipiente de três componentes com base na reacçãode imino Diels-Alder cicloadição catalisada BF3.OEt2 e sua completacaracterização estrutural foi realizada usando a técnica de difracçãocristalografia de raios X, e outros métodos espectroscópicos. A purezado produto e a composição das misturas reaccionais foram monitorizadaspor cromatografia em camada fina (CCD). Os produtos foram isoladose purificados utilizando cromatografia em coluna. As substâncias foramidentificadaos por ressonância magnética nuclear (RMN) e espectrometriade massa (EM). Os dados para caracterização por difração de raios Xforam coletados usando um Bruker AFC7S Mercury difratômetro comMo-Ka radiação (λ = 0,71073Å) à temperatura ambiente. As estruturasdosa regioisómeros foram confirmadaos por 1H RMN e 13C RMN aestrutura de cristal foi investigada usando difracção de raios X de cristalúnico. As análises espectroscópicas (RMN, EM e difracção de raios-X)demonstraram uma completa caracterização e permitiramu estabelecer aestereoquímica correcta de anel tetrahidroquinolínico. O empacotamentomolecular no cristal para 5-nitro regioisómero 4 é derivado de umacombinação de ligações de hidrogénio intermoleculares e interacções devan der Waals, e ao 7-nitro regioisómero 3 embalagens é principalmentedevido a interacções intermoleculares fracas do tipo van der Waals e N-H• • • π...

Preparation, characterization and tableting of cilnidipine solid dispersions

Solid dispersion technique has been developed many years for improving solubility of water-insoluble drugs, aiming to achieve a better oral bioavailability. However, this technique exhibits many inconveniences when used for large-scale tableting procedures. The objective of current research work was to develop cilnidipine solid dispersions [SDs] to improve the dissolution behaviors of this water-insoluble drug. Moreover, an innovative granulation method was designed to simplify the traditional tableting technology used in solid dispersion technique. Three different kinds of polymers, polyethylene glycol [PEG], polyvinylpyrrolidone [PVP] and poloxamer, were used as carriers to prepare solid dispersions. The interactions in the solid state were characterized by differential scanning calorimetry [DSC], powder Xray diffraction [PXRD] and FT-IR spectroscopy. The designed granulation method was employed to prepare solid dispersion tablets and the formulation was optimized through investigating the dissolution behaviors. The results indicated PEG solid dispersion showed the best effect both on physical characterizations and dissolution studies. Furthermore, all type of solid dispersions significantly improved the dissolution rates when compared to pure drug and its corresponding physical mixture [PM]. The solid dispersion tablets prepared in simplified tableting method exhibited better operability, stability and dissolution behavior than the tablets prepared in traditional ways, which brought more opportunities to solid dispersion technique for industrial production

Effects of ferric and chormic salts in physicochemical, surface and catalytic properties of pure and doped Fe[2]O[3]-Cr[2]O[3] system

FERRIC/CHROMIC mixed oxides having the formula 0.85 Fe[2]O[3]: 0.15 Cr[2]O[3] were obtained by thermal decomposition of the mixed hydroxides prepared from mixed nitrate and sulphate solutions using NH[4]OH. Pure mixed hydroxides were heated at 500[degree sign] C. The doped solids were prepared by treating the precipitated hydroxides with different amounts of Li[2] and K[2]O [0.5, 0.75 and 1.5 mol%] followed by calcinations at 500 [degree sign] C. The techniques employed were XRD, N[2]-adsorption and oxidation of CO by O[2] at 200-300 [degree sign] C. The results revealed that pure and doped systems consisted of nanocrystalline phases having crystallite size varying between S-64 nm depending on the nature of ferric and chromic slats used and dopant concentration. Pure mixed solids consisted of a mixture of alpha and gamma-Fe[2]O[3] phase whose crystallite size decreases by increasing the dopant concentrations. K[2]O-doping of the investigated systems resulted in the formation of K[2]FeO[4] together with ferric oxide phases. Li[2]O-doping [0.5 and 0.75 mol%] led to the formation of LiFe[5]O[8] together with gamma-Fe[2]O[3] phase. However, the heavily Li[2]O-doped samples consisted entirely of LiFe[5]O[8]. The S[BET] of pure system prepared from ferric and chromic sulphates measured higher S[BET] values as compared to those prepared from mixed nitrates, whereas K[2]O-doping decreased the S[BET]. On the other hand, Li[2]O-doping exerted a measurable increase in the S[BET]. The increase was however, more pronounced in case of the system prepared by using mixed sulphate solutions. The catalytic activity was higher in case of the catalysts prepared by using mixed nitrates as compared to the catalysts prepared by using mixed nitrates as compared to the catalysts prepared by using mixed sulphate solutions. The doping process led to a progressive significant increase in the catalytic activity. The increase was, however, much more pronounced in case of the catalysts prepared from the mixed sulphates. The maximum increase in the K[200[degree sign] C] value due to doping with 1.5 mol% K[2]O attained 20.8% and 285% for the solids prepared from mixed nitrates and mixed sulphates, respectively. These values measured 27% and 241% in case of the catalysts prepared by using mixed nitrate and mixed sulphate solutions, respectively. The doping process did not affect the mechanism of the catalyzed reaction but increased the concentrations of active sites involved in catalytic reaction without changing their energetic nature

Formulation and physicochemical characterization of piroxicam containing polymer films

Piroxicam is a potent nonsteroidal anti-inflammatory drug associated with many side effects when taken orally. An attention was paid in this work to formulate and characterize piroxicam containing polymer films for dermal use. The used polymers were Eudragit types namely Eudragit RL100, RS100, L100 and Eudragit S100. In this study, medicated films consisting of drug and carrier were prepared. The carrier consisted of one or two polymers. The physicochemical characterization was done by IR spectroscopy, DSC and X-Ray diffractometry for both piroxicam polymeric films and their corresponding physical mixtures as well as the untreated drug and polymer powders to investigate the drug polymer interaction. The results indicate presence of molecular interactions between piroxicam and both Eudragit L100 and Eudragit S100 and no interactions were found between piroxicam and Eudragit RL100 or Eudragit RS100. In-vitro drug release from Eudragit films was studied It is found that the drug release from hydrophilic polymers is faster than that from hydrophobic ones

Análises físicas e químicas de comprimidos de ecstasy apreendidos no município de São Paulo / Physical and chemical analyses of ecstasy tablets seized in São Paulo city

Drug profiling, isto é, a caracterização de amostras de drogas apreendidas no sentido de estabelecer conexões entre apreensões realizadas em diferentes épocas e/ou locais a uma origem comum de produção clandestina, tem sido um objetivo dos órgãos governamentais responsáveis pela prevenção/repressão. Especificamente tratando-se de comprimidos de ecstasy, o conhecimento de suas propriedades físicas e químicas é de relevante importância para discriminar a apreensão de diferentes lotes. Nesse contexto, o presente trabalho propõe uma nova abordagem para estabelecer conexões entre apreensões de comprimidos de ecstasy, por meio da calorimetria exploratória diferencial (DSC), termogravimetria (TG) e difratometria de raios-X (DRX). Também foi realizada a caracterização física de todos os comprimidos (logotipo, coloração, massa, diâmetro e espessura), bem como a identificação/quantificação dos constituintes ativos por cromatografia em fase gasosa acoplada à espectrometria de massas (GC-MS) e o perfil de dissolução in vitro. Além disso, foi desenvolvido um método empregando a extração líquido-líquido para o isolamento da 3,4-metilenodioximetanfetamina (MDMA) dos comprimidos de ecstasy, que posteriormente foi cristalizada para cloridrato de MDMA (MDMA.HCl). Foram analisados dezessete diferentes lotes de comprimidos de ecstasy de diversos logotipos e colorações apreendidos no município de São Paulo, Brasil. Apenas um lote apresentou como única substância ativa a clorofenilpiperazina (CPP). Os outros continham apenas MDMA e o conteúdo de MDMA variou de 29 a 115-mg/comprimido. Os valores de massa dos comprimidos variaram de 143 a 341-mg, a espessura de 3,2 a 5,8-mm e o diâmetro de 7,0 a 9,5-mm. A comparação das curvas obtidas, tanto por calorimetria exploratória diferencial (DSC) como pelos difratogramas de raios-X (DRX), permitiu discriminar aqueles com perfis semelhantes, importante para identificar a origem de produção. O baixo grau de cristalinidade do MDMA.HCl de alguns comprimidos de ecstasy não impediu a caracterização por DSC e DRX. Esses resultados podem ser úteis para a aplicação no trabalho de inteligência forense

Drug profiling or the characterization of seized drug samples to link seizures made at different times and/or locations to their common clandestine origin, has long been a goal of law enforcement agencies. Considering the trafficking of ecstasy tablets, the knowledge of chemical and physical properties is of utmost importance to discriminate between different seizures. In this context this study proposed a new approach to establish links among seizures of ecstasy tablets by using differential scanning calorimetry (DSC), thermogravimetry (TG) and X-ray diffraction (XRD). Besides this characterization, physical appearance (logotype, color, weight, diameter and thickness), identification/quantification of active constituents by gas chromatography/ mass spectrometry (GC/MS) and in vitro drug dissolution assays were performed too. A method employing liquid-liquid extraction was also developed for the isolation of 3,4-methylenedioxymethamphetamine (MDMA) from ecstasy tablets and afterwards MDMA was crystallized to MDMA hydrochloride (MDMA.HCl). Seventeen different lots of various logotypes and colors of confiscated ecstasy tablets from seizures in São Paulo city, Brazil, were analyzed. Chlorophenylpiperazine (CPP) was found only as an active ingredient in one batch. The others tablets contained only MDMA and the content of MDMA varied from 29 to 115-mg/tablet. The weight values of tablets varied from 143 to 341-mg, the thickness from 3,2 to 5,8-mm and the diameter from 7,0 to 9,5-mm. DSC/TG curves and X-ray difratograms of the ecstasy tablets allowed distinguishing those with similar profile, for both techniques, which is important to identify the source of production. The low degree of MDMA.HCl crystallinity of some ecstasy tablets didnt prevent DSC and XRD characterization. These results can be useful for forensic intelligence work application

Base catalyzed formation and ring cleavage of 2- acyl-4- alkoxycarbonyI- 4-cyano substituted cyclobexanoles

The reaction of 1, 3-diaryI-2-propen- 1 -ones [1 a, b] with ethyl cyanoacetate in absolute ethanol in the presence of a catalytic amount of KOH at 50-55°C afforded 3-aroyl-l-cyano-4-hydroxy-2,4, 6-triarylcyclohexanecarboxylates [2a,b]. Base-catalyzed ring cleavage of 2a,b in refluxing ethanolic KOH solution afforded the corresponding 3-aryl- 2-cyano-2-propenoic acid 4 along with 1 a, b. The structure of 2 was established through different spectroscopic techniques and confirmed via dehydration using thionyl chloride in refluxing pyridine afforded 3. However, reaction of la with ethyl cyanoacetate in refluxing ethanol in the presence of secondary amine [piperidine or morpholine] as a basic catalyst gave the open-chain Michael adduct 6. Treatment of the latter with ethanolic KOH solution yielded 1,5-pentanedione derivative 7. The relative configurations of 3b and 6 were determined through single crystal X-ray diffraction analysis

hydration of C3A systems in sodium chloride solutions

This study attempts to generate information about the chemistry of the hydration reaction of tricalcium aluminate [C3A] in 0.1 M sodium chloride solutions for hydration times up to one week at room temperature. The effect of gypsum, lime and alite on the progress of the reaction was investigated and the behavior of the dissolved ions was related to that of the solid phases. It is found that the hydration of C3A in 0.1 M sodium chloride solutions, also in the presence of gypsum, lime and alite has shown quite modification compared to that in water. The calcium chloro aluminate hydrate is a major phase formed in the different systems. It appears as a sole hydration product during the hydration of C3A alone in sodium chloride solutions, shows up together with ettringite phase in the presence of gypsum and predominates the ettringite phase in the presence of lime and alire. The hydration rate and the consumption of C3A in sodium chloride solution occur faster in the presence of gypsum than that in the presence of lime and alite