Development and validation of a successful microbiological agar assay for determination of ceftriaxone sodium in powder for injectable solution

Ceftriaxone sodium is a cephalosporin with broad-spectrum antimicrobial activity and belongs to the third generation of cephalosporins. Regarding the quality control of medicines, a validated microbiological assay for the determination of ceftriaxone sodium in powder for injectable solution has not been reported yet. This paper reports the development and validation of a simple, accurate and reproducible agar diffusion method to quantify ceftriaxone sodium in powder for injectable solution. The assay is based on the inhibitory effect of ceftriaxone sodium on the strain of Bacillus subtilis ATCC 9371 IAL 1027 used as test microorganism. The results were treated statistically by analysis of variance and were found to be linear (r = 0.999) in the selected range of 15.0-60.0 μg/mL, precise with a relative standard deviation (RSD) of repeatability intraday = 1.40%, accurate (100.46%) and robust with a RSD lower than 1.28%. The results demonstrated the validity of the proposed bioassay, which allows reliable ceftriaxone sodium quantitation in pharmaceutical samples and therefore can be used as a useful alternative methodology for the routine quality control of this medicine. © 2012 by the authors; licensee MDPI, Basel, Switzerland.

Physicochemical analysis of Ti-Si-B powder aalloys

Titanium alloys of Ti-Si-B system were manufactured by blended elemental powder method using Ti, Si and B powders as starting materials. It was found that uniaxial and isostatic pressing followed by hot pressing at around 1000°C, for 20 minutes, provided good densification of such alloys. The physicochemical studies were performed by means of scanning electron microscopy, X-ray diffraction, atomic force microscopy and microindentation/wear tests. The investigations revealed a multiphase microstructure formed mainly by α-titanium, Ti6Si2B, Ti5Si3, TiB and Ti3Si phases. The phase transformations after pressureless sintering at 1200°C was also studied by X-ray diffraction for the Ti-18Si-6B composition. As stated in some other researches, these intermetallics in the α-titanium matrix provide high wear resistance and hardness, with the best wear rate of 0.2 mm3/N.m and the highest hardness of around 1300 HV. © (2012) Trans Tech Publications, Switzerland.

Thermal and spectroscopic studies of solid oxamate of light trivalent lanthanides

Solid-state LnL3·1.25H2O compounds, where L is oxamate and Ln is light trivalent lanthanides, have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis, complexometry, and X-ray powder diffractometry were used to characterize and to study the thermal behavior of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, and gaseous products evolved during the thermal decomposition of these compounds in dynamic air atmosphere. The dehydration occurs in a single step and through a slow process. The thermal decomposition of the anhydrous compounds occur in a single (Ce), two (Pr), and three (La, Nd to Gd) steps with the formation of the respective oxides, CeO2, Pr 6O11, and Ln2O3 (Ln = La, Nd to Gd). The theoretical and experimental spectroscopic study suggests that the carboxylate group and amide carbonyl group of oxamate are coordinate to the metals in a bidentate chelating mode. © 2012 Akadémiai Kiadó, Budapest, Hungary.

High-density nanoparticle ceramic bodies: A study of heating rates in the sinterization of Gadolinium-doped Ceria

An investigation on the sinterization of Gd:CeO2 (Ce 0.85Gd0.15O1.9-δ ceramic system) 3-10 nm nanoparticles in pressed bodies was done. The heating rate was taken as a key parameter and two competing sinterization processes were identified, associated with different diffusional mechanisms. Using heating rates of 113 C min -1, a high-final density (98 % of the theoretical) was obtained by superposing the two aforementioned mechanisms, resulting in a homogeneous microstructure at lower temperatures. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Validation of a stability-indicating RP-LC method for the determination of tigecycline in lyophilized powder

A reversed-phase liquid chromatography (RP-LC) method was validated for the determination of tigecycline in lyophilized powder. The LC method was conducted on a Luna C18 column (250 × 4.6 mm i.d.), maintained at room temperature. The mobile phase consisted of buffer containing sodium phosphate monobasic (0.015M) and oxalic acid (0.015M) (pH 7.0)-acetonitrile (75:25, v/v), run at a flow rate of 1.0 mL/min and using ultraviolet detection at 280 nm. The chromatographic separation was obtained with a retention time of 8.6 min, and was linear in the range of 40-100 μg/mL (r2 = 0.9997). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed no interference of the excipients. The accuracy was 99.01% with a bias lower than 1.81%. The limits of detection and quantitation were 1.67 and 5.05 μg/mL, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the lyophilized powder formulation, contributing to improve the quality control and to assure the therapeutic efficacy. © The Author [2012]. Published by Oxford University Press. All rights reserved.

Photoluminescence of core-shell nanoparticles made from yttrium stabilized zirconia powder grain coated with alumina

A YSZ@Al2O3 nanocomposite was obtained by Al 2O3 coating on the surface of yttrium stabilized zirconia via a polymeric precursor method. The resulting core-shell structures were characterized by X-ray diffraction, scanning electron microscopy, transmission electronic microscopy and PL spectra. The TEM micrographs clearly show a homogeneous Al2O3 shell around the ZrO2 core. The observed PL is related to surface-interface defects. Such novel technologies can, in principle, explore materials which are not available in the bulk single crystal form but their figure-of-merit is dramatically dependent on the surface-interface defect states. © 2013 This journal isThe Royal Society of Chemistry.

Chemical composition and antioxidant activity of dried powder formulations of Agaricus blazei and Lentinus edodes

Several mushroom species have been pointed out as sources of antioxidant compounds, in addition to their important nutritional value. Agaricus blazei and Lentinus edodes are among the most studied species all over the world, but those studies focused on their fruiting bodies instead of other presentations, such as powdered preparations, used as supplements. In the present work the chemical composition (nutrients and bioactive compounds) and antioxidant activity (free radical scavenging activity, reducing power and lipid peroxidation inhibition) of dried powder formulations of the mentioned mushroom species (APF and LPF, respectively) were evaluated. Powder formulations of both species revealed the presence of essential nutrients, such as proteins, carbohydrates and unsaturated fatty acids. Furthermore, they present a low fat content (<2 g/100 g) and can be used in low-calorie diets, just like the mushrooms fruiting bodies. APF showed higher antioxidant activity and higher content of tocopherols and phenolic compounds (124 and 770 μg/100 g, respectively) than LPF (32 and 690 μg/100 g). Both formulations could be used as antioxidant sources to prevent diseases related to oxidative stress. © 2012 Elsevier Ltd. All rights reserved.

The reactive surface of Castor leaf [Ricinus communis L.] powder as a green adsorbent for the removal of heavy metals from natural river water

In this study, a green adsorbent was successfully applied to remove toxic metals from aqueous solutions. Dried minced castor leaves were fractionated into 63-μm particles to perform characterization and extraction experiments. Absorption bands in FTIR (Fourier Transform Infrared Spectroscopy) spectra at 1544, 1232 and 1350 cm-1 were assigned to nitrogen-containing groups. Elemental analysis showed high nitrogen and sulfur content: 5.76 and 1.93%, respectively. The adsorption kinetics for Cd(II) and Pb(II) followed a pseudo-second-order model, and no difference between the experimental and calculated Nf values (0.094 and 0.05 mmol g-1 for Cd(II) and Pb(II), respectively) was observed. The Ns values calculated using the modified Langmuir equation, 0.340 and 0.327 mmol g-1 for Cd(II) and Pb(II), respectively, were superior to the results obtained for several materials in the literature. The method proposed in this study was applied to pre-concentrate (45-fold enrichment factor) and used to measure Cd(II) and Pb(II) in freshwater samples from the Paraná River. The method was validated through a comparative analysis with a standard reference material (1643e). © 2013 Elsevier B.V. © 2013 Elsevier B.V. All rights reserved.

Synthesis, structural characterization and photophysical properties of highly photoluminescent crystals of Eu(III), Tb(III) and Dy(III) with 2,5-thiophenedicarboxylate

Lanthanide compounds of general formula [Ln2(2,5-tdc) 3(dmf)2(H2O)2] ·2dmf·H2O (Ln = Eu(III) (1), Tb(III) (2), Gd(III) (3) and Dy(III) (4), dmf = N,N′-dimethylformamide and 2,5-tdc2- = 2,5-thiophedicarboxylate anion) were synthesized and characterized by elemental analysis, X-ray powder diffraction patterns, thermogravimetric analysis and infrared spectroscopy. Phosphorescence data of Gd(III) complex showed that the triplet states (T1) of 2,5-tdc2- ligand have higher energy than the main emitting states of Eu(III), Tb(III) and Dy(III), indicating that 2,5-tdc2- ligand can act as intramolecular energy donor for these metal ions. An energy level diagram was used to establish the most relevant channels involved in the ligand-to-metal energy transfer. The high value of experimental intensity parameter Ω2 for the Eu(III) complex indicate that the europium ion is in a highly polarizable chemical environment. The emission quantum efficiency (η) of the 5D0 emitting level of Eu(III) was also determined. The complexes act as possible light conversion molecular devices (LCMDs). © 2013 Elsevier B.V. All rights reserved.

A ressonância magnética no estudo da desintegração de comprimidos marcados com açaí (Euterpe oleracea)

Pós-graduação em Biologia Geral e Aplicada - IBB

Fabricação e caracterização de fios supercondutores do sistema BSCCO pelo método Powder-In-Tube (PIT)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Propriedades e mecanismos de cintilação dos materiais 'GD''AL''O IND.3' e ('GD''LU')'AL''O IND.3' dopados com 'EU POT. 3+', 'TB POT. 3+' e 'PR POT. 3+'

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Cinética de sinterização do combustível nuclear 'UO IND. 2.'7%'Gd IND.2''O IND. 3': cálculo da curva mestre de sinterização

Pós-graduação em Ciência e Tecnologia de Materiais - FC

Síntese, caracterização e estudo do comportamento térmico dos 2-clorobenzalpiruvatos de lantânio (III), lantanídios (III) e de ítrio (III), no estado sólido

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Luminescência e aspectos estruturais de difenilfosfinatos de alguns íons lantanídeos

Pós-graduação em Química - IQ