Inclusion complex of the antiviral drug acyclovir with cyclodextrin in aqueous solution and in solid phase

Complexation between acyclovir (ACV), an antiviral drug used for the treatment of herpes simplex virus infection, and beta-cyclodextrin (beta-CD) was studied in solution and in solid states. Complexation in solution was evaluated using solubility studies and nuclear magnetic resonance spectroscopy (¹H-NMR). In the solid state, X-ray diffraction, differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA) and dissolution studies were used. Solubility studies suggested the existence of a 1:1 complex between ACV and beta-CD. ¹H-NMR spectroscopy studies showed that the complex formed occurs with a stoichiometry ratio of 1:1. Powder X-ray diffraction indicated that ACV exists in a semicrystalline state in the complexed form with beta-CD. DSC studies showed the existence of a complex of ACV with beta-CD. The TGA studies confirmed the DSC results of the complex. Solubility of ACV in solid complexes was studied by the dissolution method and it was found to be much more soluble than the uncomplexed drug.

Estudo termogravimétrico e calorimétrico da algaroba

Humidity and ash content of powder and bran of algaroba pods are important quality parameters for biological control during storage. The studies of humidity and ash content were carried out conventional and thermogravimetric methods. Different values were obtained by the various methods. The thermogravimetric method was faster and required less sample for the humidity and ash analyses of the powder and bran of algaroba pods. The differential scanning calorimetry curves of the powder and bran of algaroba pods, dryed at 55 ºC, showed two peaks, one corresponding to the gelatinization of starch and the other to the vaporization of water. The samples dryed at 65, 75, 85, 95 and 105 ºC showed one peak, corresponding to the vaporization of water.

Propelente sólido compósito polibutadiênico: I- influência do agente de ligação

In the Brazilian Complete Spacial Mission, the research of Vehicle Satellite Launcher is important. The solid propellant composite used in this vehicle is made with ammonium perchlorate, aluminiun powder and hydroxy terminated polibutadiene resin. In the propellant the bonding agent has a function to promote the interaction between solids and polimeric matrix, improving mechanical properties as stress, strain, aging characteristics and moisture embrittlement. Due its importance in propellant, bonding agent is consider as industrial secret and the literature about it is generic, without greater informations.

A new experimental procedure to obtain titania powders as anatase phase by a sol-gel process

Titania powders were synthesized by a sol-gel process using titanium tetrabutoxide as precursor. The syntheses were performed in water or in solutions of dimethylformamide (dmf) or dimethylsulfoxide (dmso). It is demonstrated, by X-ray diffraction patterns of the synthesized powders, that the samples obtained in dmf or dmso solutions are crystalline (anatase phase) with some minor amount of brookite phase, whereas the sample synthesized in water is amorphous. The anatase phase can be obtained independently of any previous or further treatment of the synthesized powder, such as hydrothermal or heat treatment, providing a new, simple, quick and inexpensive route to synthesize anatase powders. From the peak broadening of the anatase (101) diffraction, the crystallite sizes were calculated as 6 nm.

Comportamento térmico da caulinita hidratada

Well-ordered kaolinite from the Brazilian Amazon Region (State of Pará) was initially reacted at 60 °C with a water dimethylsulfoxide mixture. After washing and characterisation, the resulting material was washed several times with methanol and in the final step with water. The water molecules displace the previously dimethylsulfoxide intercalated molecules and two different hydrated kaolinites were obtained. An unstable phase characterized by an interplanar basal distance of 0,996 nm that after drying collapse to the stable 0,844 nm hydrated kaolinite. The dehydration of the sample to disordered kaolinite was accompanied by Powder X-ray Diffractometry, thermal analysis (simultaneous TG and DSC) and FTIR spectroscopy.

A extração de cafeína em bebidas estimulantes: uma nova abordagem para um experimento clássico em química orgânica

Caffeine extraction procedures from water soluble and water insoluble materials for preparing stimulating beverages are described. Water soluble materials used were instant tea and coffee and water insoluble materials were, among others, guaraná powder and maté leaves. The extraction of caffeine from water soluble materials, especially instant tea, is more suitable for an organic chemistry teaching laboratory than the classic experiment using tea leaves, due to the economy of time and a larger amount of extracted caffeine. The procedure is time-saving and requires only a four-hour period. The experiments illustrate the extraction process as used in undergraduate organic chemistry laboratories.

Óxidos de ferro magnéticos de um tufito da região do Alto Paranaíba, MG

The Mössbauer analysis along with the structural Rietveld refinement based on powder X-ray data for the magnetic fraction (saturation magnetization, sigma = 19 J T-1 kg-1) separated from a tuffite material from Alto Paranaíba, state of Minas Gerais, Brazil, reveal that a (Ti, Mg)-rich maghemite (deduced sigma = 17 J T-1 kg-1) and, for the first time observed in this lithodomain, magnesioferrite (characteristic sigma = 21 J T-1 kg-1) respond for the magnetization of the rock material. Consistent models for the ionic distribution in these iron-rich spinel structures are proposed.

Preparação de compostos lamelares: síntese do hidrogenofosfato de zircônio cristalino e sua intercalação com aminas. Um experimento para estudantes de graduação

The present paper describes the synthesis of crystalline zirconium hydrogen phosphate by direct precipitation and its intercalation with pyridine and n-butylamine. The simple experiment was tested in the undergraduate inorganic chemistry laboratory course for chemistry students at IQ-UNICAMP using inexpensive reagents. The materials were characterized by powder X-ray diffraction and infrared analyses in order to obtain detailed information of the solid structure changes as a result of the intercalation process. Pyridine and n-butylamine are focused in this work as clear and elucidative examples leading to acid-base interactive processes that result in the well-formed infinite sequence of inorganic lamellar structures.

Los electrodos de pasta de carbono en el estudio electroquímico de minerales metálicos

This paper shows the applicability of the carbon paste electrode-mineral (CPE-mineral) to study the dissolution mechanisms of minerals in powder form and in flotation concentrates. A potentiodynamic strategy to find the dissolution mechanism of galena (PbS) is presented. In this way, minerals less studied such as orpiment (As2S3) and realgar (As2S2) are investigated. The electrochemical activity of a more complicated mineral such as sphalerite (ZnS), containing 12.3 and 0.43% of iron in solid solution, is discussed. The mechanism of a complex zinc concentrate (containing 63.4% ZnS, 20.1% FeS2, 5% CuFeS2, 0.33% PbS, 0.45% Cu12Sb4S13 and 0.4% FeAsS) is described. Finally, an electrochemical method for the detection of the different leachable and refractory silver phases (contained in two mineral concentrates) is presented. This paper reviews the power of the use of CPE-mineral coupled to electrochemical techniques in hydrometallurgy.

Estudo do efeito do tratamento superficial por moagem sobre as propriedades das partículas de uma liga de hidreto metálico

This work reports results of studies on the electrochemical and structural properties of a Ti/Zr-based metal hydride alloy covered by Ni and LaNi4,7Sn0,3 powder additives by ball milling. The effect of this treatment is investigated for the activation time, hydrogen storage capacity and equilibrium pressure, cycling stability and the hydration/dehydration kinetics. Charge and discharge cycles show a significant decrease of the activation time due to an increase of the active area caused by the milling treatment, independent of the additive. However, other results have evidenced little effect of the milling surface treatment on the charge storage capacity, hydrogen equilibrium pressure, and hydration/dehydration kinetics, for both the Ni and LaNi4,7Sn0,3 covered materials.

Espectrofotometria derivativa: uma estratégia simples para a determinação simultânea de corantes em alimentos

A very simple spectrophotometric method is described for resolving binary mixture of the food colorants Sunset Yellow (INS 110) and Tartrazine Yellow (INS 102) by using the first derivative spectra with measurements at zero-crossing wavelengths. Before the spectrophotometric measurements, the dyes were sorbed onto polyurethane foam and recovered in N,N-dimethilformamide. Commercial food products (gelatine and juice powder) were analysed by using the proposed method and the HPLC technique. The results are in very good agreement and the differences between the methods is not statistically important. Therefore, the first-order derivative spectrophotometric method is accurate, precise, reliable and could be applied to the routine analysis of food samples.

Taninos hidrolisáveis em Bixa orellana L.

The aqueous material found in the fruits of Bixa Orellana L. was collected, dried, and characterized using several experimental techniques, namely phytochemical analysis in order to identify the biologically active constituents, Fourier transform infrared (FT-IR) spectroscopy for vibrational analysis, and X-ray powder diffraction in order to identify the presence of crystalline phases in the sample. The results showed that the aqueous material possesses high concentrations of hydrolyzable tannin. This result justifies the anti-inflammatory activity of this substance reported in other studies.

Determinação de resíduos de cloranfenicol em amostras de leite e mel industrializados utilizando a técnica de espectrometria de massas em "tandem" (CLAE-EM/EM)

The present work shows a method for the determination of chloramphenicol (CAP) antibiotic in milk, powder milk and honey. The solid phase extraction and liquid-liquid extraction were applied as a clean-up and pre-concentration strategies followed by LC-ESI/MS/MS analysis. The recovery was studied for different fortification levels from 0.05 to 1.00 µg L-1 in milk, showing values between 91 101% and RSD bellow 8.0%, while honey was spiked with a concentration of 0.20 µg kg-1 yelding a mean recovery of 83% and RSD of 6.5%. The quantification transition 321>152 showed a LOD of 0.52 ng kg-1 and LOQ of 1.85 ng kg-1.

Análises quali- e quantitativa de cafés comerciais via ressonância magnética nuclear

Coffee is one of the beverages most widely consumed in the world and the "cafezinho" is normally prepared from a blend of roasted powder of two species, Coffea arabica and Coffea canephora. Each one exhibits differences in their taste and in the chemical composition, especially in the caffeine percentage. There are several procedures proposed in the literature for caffeine determination in different samples like soft drinks, coffee, medicines, etc but most of them need a sample workup which involves at least one step of purification. This work describes the quantitative analysis of caffeine using ¹H NMR and the identification of the major components in commercial coffee samples using 1D and 2D NMR techniques without any sample pre-treatment.

Caracterização espectroscópica de peixe do período cretáceo (Bacia do Araripe)

The study of fossils has made considerable progress over the last years as a result of the use of new experimental techniques. This paper describes the chemical composition of a fossilized fish of the Cretaceous period, from a 100 million-year-old, material originated from the Araripe Basin (northeastern Brazil). The chemical composition of the fossilized fish was analyzed by means of X-ray powder diffraction and Fourier transform infrared spectroscopy (FT-IR). The spectroscopic study has proven that the main substances found in the fossilized fish are CaCO3 and Ca5(PO4)3(OH). A tentative mechanism to explain the fossilization process is also given.