Development of a new high-performance liquid chromatographic method for the determination of ceftazidime

A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanol-water (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 mu g/mL. The values for interday and intraday precision (relative standard deviation) were < 1 %. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Development and validation of a new and rapid HPLC for determination of lyophilized teicoplanin

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Caracterização anatômica e fitoquímica de folhas e rizomas de Hedychium coronarium J. König (Zingiberaceae)

Devido a grande potencialidade na utilização de Hedychium coronarium, na medicina popular e também como biorremediadora no tratamento de efluentes, objetivou-se uma diagnose dos órgãos, folha e rizoma, para elucidar resultados estruturais e fitoquímicos. A folha é anfiestomática, com predominância de estômatos na face abaxial. em ambas as superfícies foliares há projeções de cera epicuticular sobre as paredes anticlinais das células epidérmicas. O mesofilo dorsiventral apresenta hipoderme multisseriada (3 camadas) em ambos os lados. O parênquima clorofiliano é diferenciado em paliçádico (1-2 camadas) e lacunoso (4-5 camadas) com muitos espaços intercelulares e ocorrência de idioblastos cristalíferos. Na nervura central, o aerênquima ocorre em único arco na região abaxial. Os feixes vasculares distribuem-se aleatoriamente e são de diferentes tamanhos, pequenos, médios e grandes, envolvidos por fibras. Os feixes menores localizam-se no lado abaxial da nervura. A triagem fitoquímica das folhas mostrou a presença de saponinas e ausência de taninos, antraquinonas, alcalóides e flavonóides. Por meio de Cromatografia em Camada Delgada foram identificadas as presenças de cariofileno e mirceno no óleo essencial bruto obtido a partir das folhas de H. coronarium.

Desempenho de reatores aeróbios de leito fluidizado com circulação interna na remoção de matéria carbonácea tratando diferentes águas residuárias

The organic matter. (OM) removal efficiency in the biochemical oxygen demand (BOD) and chemical oxygen demand (COD) forms for domestic wastewater and semi-intensive fish culture effluents by using three phase aerobic fluidized bed reactors with circulation in concentric tubes was studied. Three different ratios between external and internal areas by different internal diameter configurations (100, 125 and 150mm) to the same external diameter of 250mm were used; sand for filters and granulated activated carbon were used as supporting media. The reactors were tested for three hydraulic retention times: 11.5min to the R100, and 3h for the R125 and R150 reactors. The results demonstrated that this kind of reactors had good performance in the BOD and COD removal for different concentrations of waste waters. BOD mean removal efficiencies obtained were: 47% at the R100 reactor, 57% and 93% of raw and filtered BOD respectively at R125, 48 and 89% of raw and filtered BOD at R150. The COD mean calculated removal efficiencies were: 75% at the R100 reactor, 56 and 86% of raw and filtered COD at R125, and 54 and 86% of raw and filtered COD at R150. In the case of domestic wastewater it is necessary to provide a solids removal system at the reactor outflow in order to increase the removal of suspended OM from the final effluent.

Hydrodynamic characterization and performance evaluation of an aerobic three phase airlift fluidized bed reactor in a recirculation aquaculture system for Nile Tilapia production

The hydrodynamic characterization and the performance evaluation of an aerobic three phase fluidized bed reactor in wastewater fish culture treatment are presented in this report. The objective of this study was to evaluate the organic matter, nitrogen and phosphorous removal efficiency in a physical and biological wastewater treatment system of an intensive Nile Tilapia laboratory production with recirculation. The treatment system comprised of a conventional sedimentation basin operated at a hydraulic detention time HDT of 2.94 h and an aerobic three phase airlift fluidized bed reactor AAFBR operated at an 11.9 min HDT. Granular activated carbon was used as support media with density of 1.64 g/cm(3) and effective size of 0.34 mm in an 80 g/L constant concentration. Mean removal efficiencies of BOD, COD, phosphorous, total ammonia nitrogen and total nitrogen were 47%, 77%, 38%, 27% and 24%, respectively. The evaluated system proved an effective alternative for water reuse in the recirculation system capable of maintaining water quality characteristics within the recommended values for fish farming and met the Brazilian standards for final effluent discharges with exception of phosphorous values. (C) 2011 Elsevier B.V. All rights reserved.

Monitoramento de 24 horas do desempenho de reator aeróbio de leito fluidizado trifásico na remoção de amônio num sistema de recirculação para produção de tilápia

O objetivo deste trabalho foi monitorar o desempenho de remoção de nitrogênio amoniacal no tratamento das águas residuárias da produção intensiva de tilápia nilótica em sistema com recirculação de água. O sistema foi constituído por um sedimentador convencional e um reator aeróbio de leito fluidizado trifásico com circulação, operados com tempos de detenção hidráulica de 176.4 e 11.9 minutos respectivamente. O meio suporte utilizado no reator foi o carvão ativado granular com densidade aparente de 1.64 g/cm3 e tamanho efetivo de 0.34 mm; a concentração do meio suporte no reator foi mantida constante em 80 g/L. A eficiência média de remoção do nitrogênio amoniacal total foi de 41.2%. O sistema avaliado é uma alternativa efetiva para o reuso da água em sistemas de recirculação para aqüicultura. Embora a variabilidade das concentrações do nitrogênio amoniacal afluente cujo valor médio foi de 0.136 mg/L, o efluente do reator conservou as características de qualidade da água estáveis, com concentrações médias de nitrogênio amoniacal de 0.079 mg/L e do oxigênio dissolvido de 6.70 mg/L, recomendáveis para a criação dos peixes e nas faixas de valores permitidos pela legislação Brasileira (Resolução CONAMA No. 357 de março 5 de 2005) para lançamento de efluentes finais nos corpos de água receptores.

Análise dos Processos de Flotação e Oxidação Avançada para o Tratamento de Efluente Modelo da Indústria do Petróleo

The generation of wastes in most industrial process is inevitable. In the petroleum industry, one of the greatest problems for the environment is the huge amount of produced water generated in the oil fields. This wastewater is a complex mixture and present great amounts. These effluents can be hazardous to the environmental without adequate treatment. This research is focused in the analysis of the efficiencies of the flotation and photo-oxidation processes to remove and decompose the organic compounds present in the produced water. A series of surfactants derivated from the laurilic alcohol was utilized in the flotation to promote the separation. The experiments have been performed with a synthetic wastewater, carefully prepared with xylene. The experimental data obtained using flotation presented a first order kinetic, identified by the quality of the linear data fitting. The best conditions were found at 0.029 g.L-1 for the surfactant EO 7, 0.05 g.L-1 for EO 8, 0.07 g.L-1 for EO 9, 0.045 g.L-1 for EO 10 and 0.08 g.L-1 for EO 23 with the following estimated kinetic constants: 0.1765, 0.1325, 0.1210, 0.1531 and 0.1699 min-1, respectively. For the series studied, the most suitablesurfactant was the EO 7 due to the lower reagent consumption, higher separation rate constant and higher removal efficiency of xylene in the aqueous phase (98%). Similarly to the flotation, the photo-Fenton process shows to be efficient for degradation of xylene and promoting the mineralization of the organic charge around 90% and 100% in 90 min

Tratamento eletroquímico de água produzida sintética para remoção de hidrocarbonetos policíclicos aromáticos

The aim of this work is the treatment of produced water from oil by using electrochemical technology. Produced water is a major waste generated during the process of exploration and production in the oil industry. Several approaches are being studied aiming at the treatment of this effluent; among them can be cited the biological process and chemical treatments such as advanced oxidation process and electrochemical treatments (electrooxidation, electroflotation, electrocoagulation, electrocoagulation). This work studies the application of electrochemical technology in the treatment of the synthetic produced water effluent through the action of the electron, in order to remove or transform the toxic and harmful substances from the environment by redox reactions in less toxic substances. For this reason, we used a synthetic wastewater, containing a mixture H2SO4 0,5M and 16 HPAs, which are: naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, chrysene, benzo(b)fluoranthene, benzo(k) fluoranthene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a, h)anthracene, benzo(g, h, i)perylene. Bulk electrochemical oxidation experiments were performed using a batch electrochemical reactor containing a pair of parallel electrodes, coupled with a power supply using a magnetic stirrer for favoring the transfer mass control. As anodic material was used, a Dimensionally Stable Anode (DSA) of Ti/Pt, while as cathode was used a Ti electrode. Several samples were collected at specific times and after that, the analysis of these samples were carried out by using Gas Chromatography Coupled to Mass Spectrometry (GC - MS) in order to determine the percentage of removal. The results showed that it was possible to achieve the removal of HPAs about 80% (in some cases, more than 80%). In addition, as an indicator of the economic feasibility of electrochemical treatment the energy consumption was analyzed for each hour of electrolysis, and based on the value kWh charged by ANEEL, the costs were estimated. Thus, the treatment costs of this research were quite attractive

Utilização de microemulsão na remoção da cor de efluentes têxteis contendo corantes dispersos

Polyester fibers are the most used fibers in the world and disperse dyes are used for dyeing these fibers. After dyeing, the colorful dyebath is discharged into effluent streams, which needs a special treatment for color removal. Surfactants interaction with dyes has been evaluated in several studies, including the textile area, specifically in the separation of dyes from textile wastewater. In this work a cationic surfactant was used in a microemulsion system for the extraction of anionic dyes (disperses dyes) from textile wastewater. These microemulsion system was composed by dodecylamonium chloride (surfactant), kerosene oil (organic phase), isoamyl alcohol (cosurfactant) and the wastewater (aqueous phase). The wastewater that results after the dyeing process is acid (pH 5). It was observed that changing the pH value to above 12.8 the extraction could be made, resulting in an aqueous phase with low color level. The Scheffé net experimental design was used for the extraction process optimization, and the obtained results were evaluated using the program "Statistica 7.0". The optimal microemulsion system was composed by 59.8wt.% of wastewater, 30.1wt.% of kerosene, 3.37wt.% of surfactant and 6.73wt.% of cosurfactant, providing extraction upper than 96%. A mix of reactive dyebath (50%) and disperse dyebath (50%) was used as aqueous phase and it presented extraction upper than 98%. The water phase after extraction process can be reused in a new dyeing, being obtained satisfactory results, according to the limits established by textile industry for a good dyeing. Tests were accomplished seeking to study the influence of salt addition and temperature. An experimental design was used for this purpose, which showed that the extraction doesn't depend on those factors. In this way, the removal of color from textile wastewater by microemulsion is a viable technique (that does not depend of external factors such as salinity and temperature), being obtained good extraction results even with in wastewater mixtures

Tecnologia eletroquímica como tratamento alternativo de efluentes têxteis sintéticos utilizando ânodos de platina e diamante

In this work, the treatment of synthetic wastewaters containing Remazol Red BR (RRB) and Novacron Blue C-D (NB) by anodic oxidation using boron doped diamond anodes (BDD) and Novacron Yellow (YN) using BDD and Platinum (Pt) anodes was investigated. Galvanostatic electrolyses of RRB and NB synthetic wastewaters have led to the complete decolorization removal at different operating conditions (current density, pH and temperature). The influence of these parameters was investigated in order to find the best conditions for dyestuff colour removal. According to the experimental results obtained, the electrochemical oxidation process is suitable for decolorizing wastewaters containing these textile dyes, due to the electrocatalytic properties of BDD and Pt anode. Energy requirements for removing colour during galvanostatic electrolyses of RRB, NB and YN synthetic solutions depends mainly on the operating conditions; for example for RRB, it passes from 3.30 kWh m-3 at 20 mA cm-2 to 4.28 kWh m-3 at 60 mA cm-2 (pH = 1); 15.23 kWh m-3 at 20 mA cm-2 to 24.75 kWh m-3 at 60 mA cm-2 (pH = 4.5); 10.80 kWh m-3 at 20 mA cm-2 to 31.5 kWh m-3 at 60 mA cm-2 (pH = 8) (data estimated per volume of treated effluent). In order to verify the Brazilian law regulations of NB and RRB synthetic solutions after electrochemical decolourisation treatment, Hazen Units values were determined and the total colour removal was achieved; remaining into the regulations. Finally, electrical energy cost for removing colour was estimated

Aplicação da tecnologia eletroquímica como alternativa para a remoção de corante têxteis em efluentes sintéticos e reais utilizando anodos de platina e diamante

In this work, electrochemical technology was used to treat synthetic wastewater containing Methyl Red (MR) and Blue Novacron (BN) by anodic oxidation using anodes platinum (Pt) and real samples of textile effluents using DDB anodes and platinum (Pt). The removal of color from the galvanostatic electrolysis of synthetic wastewater MR and BN, and the actual sample has been observed under different conditions (different current densities and temperature variation). The investigation of these parameters was performed in order to establish the best conditions for removal of color and chemical oxygen demand (BOD). According to the results obtained in this study, the electrochemical oxidation processes suitable for the degradation process of color and COD in wastewater containing such textile dyes, because the electrocatalytic properties of Pt and BDD anodes consumption energy during the electrochemical oxidation of synthetic solutions AN and MR and real sample, mainly depend on the operating parameters of operation, for example, the synthetic sample of MR, energy consumption rose from 42,00kWhm-3 in 40 mAcm-2 and 25 C to 17,50 kWhm-3 in 40mAcm-2 and 40 C, from the BN went 17,83 kWhm-3 in 40mAcm and 40°C to 14,04 kWhm- 3 in 40mAcm-2 and 40 C (data estimated by the volume of treated effluent). These results clearly indicate the applicability of electrochemical treatment for removing dyes from synthetic solutions and real industrial effluents

Avaliação da poatencialidade da perlita natural e expandida na adsorção de metais

The contamination by metal ions has been occurring for decades through the introduction of liquid effluent not treated, mainly from industrial activities, rivers and lakes, affecting water quality. For that the effluent can be disposed in water bodies, environmental standards require that they be adequately addressed, so that the concentration of metals does not exceed the limits of standard conditions of release in the receptor. Several methods for wastewater treatment have been reported in the literature, but many of them are high cost and low efficiency. The adsorption process has been used as effective for removal of metal ions. This paper presents studies to evaluate the potential of perlite as an adsorbent for removing metals in model solution. Perlite, in its natural form (NP) and expanded (EP), was characterized by X-ray fluorescence, X-ray diffraction, surface area analysis using nitrogen adsorption (BET method), scanning electron microscopy and Fourier transform infrared spectroscopy. The physical characteristic and chemical composition of the material presented were appropriate for the study of adsorption. Adsorption experiments by the method of finite bath for model solutions of metal ions Cr3+, Cu2+, Mn2+ and Ni2+ were carried out in order to study the effect of pH, mass of the adsorbent and the contact time on removal of ions in solution. The results showed that perlite has good adsorption capacity. The NP has higher adsorption capacity (mg g-1) than the EP. According to the values of the constant of Langmuir qm (mg g-1), the maximum capacity of the monolayer was obtained and in terms of proportion of mass, we found the following order experimental adsorption: Cr3+ (2.194 mg g- 1) > Ni2+ (0.585 mg g-1) > Mn2+ (0.515 mg g-1) > Cu2+ (0.513 mg g-1) and Cr3+ (1.934 mg g-1)> Ni2+ (0.514 mg g-1) > Cu2+ (0.421 mg g-1) > Mn2+ (0.364 mg g-1) on the NP and EP, respectively. The experimental data were best fitted the Langmuir model compared to Freundlich for Cu2+, Mn2+ and Ni2+. However, for the Cr3+, both models fit the experimental data

Degradação eletroquímica de benzeno, tolueno e xileno via oxidação eletroquímica utilizando eletrodo Ti/Pt

This work is directed to the treatment of organic compounds present in produced water from oil using electrochemical technology. The water produced is a residue of the petroleum industry are difficult to treat , since this corresponds to 98 % effluent from the effluent generated in the exploration of oil and contains various compounds such as volatile hydrocarbons (benzene, toluene, ethylbenzene and xylene), polycyclic aromatic hydrocarbons (PAHs), phenols, carboxylic acids and inorganic compounds. There are several types of treatment methodologies that residue being studied, among which are the biological processes, advanced oxidation processes (AOPs), such as electrochemical treatments electrooxidation, electrocoagulation, electrocoagulation and eletroredution. The electrochemical method is a method of little environmental impact because instead of chemical reagents uses electron through reactions of oxide-reducing transforms toxic substances into substances with less environmental impact. Thus, this paper aims to study the electrochemical behavior and elimination of the BTX (benzene, toluene and xylene) using electrode of Ti/Pt. For the experiment an electrochemical batch system consists of a continuous source, anode Ti/Pt was used, applying three densities of current (1 mA/cm2, 2,5 mA/cm2 and 5 mA/cm2). The synthetic wastewater was prepared by a solution of benzene, toluene and xylene with a concentration of 5 ppm, to evaluate the electrochemical behavior by cyclic voltammetry and polarization curves, even before assessing the removal of these compounds in solution by electrochemical oxidation. The behavior of each of the compounds was evaluated by the use of electrochemical techniques indicate that each of the compounds when evaluated by cyclic voltammetry showed partial oxidation behavior via adsorption to the surface of the Ti/Pt electrode. The adsorption of each of the present compounds depends on the solution concentration but there is the strong adsorption of xylene. However, the removal was confirmed by UV-Vis, and analysis of total organic carbon (TOC), which showed a percentage of partial oxidation (19,8 % - 99,1 % TOC removed), confirming the electrochemical behavior already observed in voltammetry and cyclic polarization curves

Encapsulação de nanopartículas de magnetita em matriz de poli(metacrilato de metilacoácido metacrílico) por processo de polimerização em miniemulsão

Magnetic particles are systems with potential use in drug delivery systems, ferrofluids, and effluent treatment. In many situations, such as in biomedical applications, it is necessary to cover magnetic particles with an organic material, as polymers. In this work, magnetic particles were obtained through covering magnetite particles with poly(methyl methacrylate‐comethacrylic acid) via miniemulsion polymerization process. The resultant materials were characterized X‐ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), zeta potential (��) measurements and vibrating sample magnetometry (VSM). XRD results showed magnetite as the predominant cristalline phase in all samples and that cristallites had nanometric dimensions. Thermogravimetric analysis revealed an increase in polymer thermal stability as a result of magnetite encapsulation. TGA results showed also that the encapsulation efficiency was directly related to nanoparticles s hidrofobicity degree. VSM measurements showed that magnetic polymeric particles were superparamagnetic, so that they may be potentially used for magnetic (bio)separation

Caracterização química e toxicológica da água produzida descartada em plataformas de óleo e gás na costa brasileira e seu comportamento dispersivo no mar

The production of oil and gas is usually accompanied by the production of water, also known as produced water. Studies were conducted in platforms that discharge produced water in the Atlantic Ocean due to oil and gas production by Petrobras from 1996 to 2006 in the following basins: Santos (Brazilian south region), Campos (Brazilian southeast region) and Ceara (Brazilian northeast region). This study encompasses chemical composition, toxicological effects, discharge volumes, and produced water behavior after releasing in the ocean, including dispersion plumes modeling and monitoring data of the marine environment. The concentration medians for a sampling of 50 samples were: ammonia (70 mg L-1), boron (1.3 mg L1), iron (7.4 mg L-1), BTEX (4.6 mg L-1), PAH (0.53 mg L-1), TPH (28 mg L-1); phenols (1.3 mg L-1) and radioisotopes (0.15 Bq L-1 for 226Ra and 0.09 Bq L-1 for 228Ra). The concentrations of the organic and inorganic parameters observed for the Brazilian platforms were similar to the international reference data for the produced water in the North Sea and in other regions of the world. It was found significant differences in concentrations of the following parameters: BTEX (p<0.0001), phenols (p=0.0212), boron (p<0.0001), iron (p<0.0001) and toxicological response in sea urchin Lytechinus variegatus (p<0.0001) when considering two distinguished groups, platforms from southeast and northeast Region (PCR-1). Significant differences were not observed among the other parameters. In platforms with large gas production, the monoaromatic concentrations (BTEX from 15.8 to 21.6 mg L-1) and phenols (from 2 to 83 mg L-1) were higher than in oil plataforms (median concentrations of BTEX were 4.6 mg L-1 for n=53, and of phenols were 1.3 mg L-1 for n=46). It was also conducted a study about the influence of dispersion plumes of produced water in the vicinity of six platforms of oil and gas production (P-26, PPG-1, PCR-1, P-32, SS-06), and in a hypothetical critical scenario using the chemical characteristics of each effluent. Through this study, using CORMIX and CHEMMAP models for dispersion plumes simulation of the produced water discharges, it was possible to obtain the dilution dimension in the ocean after those discharges. The dispersion plumes of the produced water modelling in field vicinity showed dilutions of 700 to 900 times for the first 30-40 meters from the platform PCR-1 discharge point; 100 times for the platform P-32, with 30 meters of distance; 150 times for the platform P-26, with 40 meters of distance; 100 times for the platform PPG-1, with 130 meters of distance; 280 to 350 times for the platform SS-06, with 130 meters of distance, 100 times for the hypothetical critical scenario, with the 130 meters of distance. The dilutions continue in the far field, and with the results of the simulations, it was possible to verify that all the parameters presented concentrations bellow the maximum values established by Brazilian legislation for seawater (CONAMA 357/05 - Class 1), before the 500 meters distance of the discharge point. These results were in agreement with the field measurements. Although, in general results for the Brazilian produced water presented toxicological effects for marine organisms, it was verified that dilutions of 100 times were sufficient for not causing toxicological responses. Field monitoring data of the seawater around the Pargo, Pampo and PCR-1 platforms did not demonstrate toxicity in the seawater close to these platforms. The results of environmental monitoring in seawater and sediments proved that alterations were not detected for environmental quality in areas under direct influence of the oil production activities in the Campos and Ceara Basin, as according to results obtained in the dispersion plume modelling for the produced water discharge