Estudo comparativo de diferentes sistemas de injeção de vapor aplicados à remediação de solos contaminados por diesel

Among the potentially polluting economic activities that compromise the quality of soil and groundwater stations are fuel dealers. Leakage of oil derived fuels in underground tanks or activities improperly with these pollutants can contaminate large areas, causing serious environmental and toxicological problems. The number of gas stations grew haphazardly, without any kind of control, thus the environmental impacts generated by these enterprises grew causing pollution of soil and groundwater. Surfactants using various techniques have been proposed to remedy this kind of contamination. This study presents innovation as the application of different systems containing surfactant in the vapor phase and compares their diesel removal efficiencies of soil containing this contaminant. For this, a system that contains seven injection wells the following vaporized solutions: water, surfactant solution, microemulsion and nanoemulsion, The surfactants used were saponified coconut oil (OCS), in aqueous solution and an ethoxylated alcohol UNTL-90: aqueous solution , and nanoemulsion and microemulsion systems. Among the systems investigated, the nanoemulsion showed the highest efficiency, achieving 88% removal of residual phase diesel, the most ecologically and technically feasible by a system with lower content of active matter

Otimização da extração de polissacarídeos sulfatados da alga vermelha Gracilaria birdiae e análise da atividade anticoagulante e antioxidante

The sulfated polysaccharides (SP) from the edible red seaweed Gracilaria birdiae were obtained using five different condition extraction (GB1: Water; GB1p: Water/proteolysis; GB1s: Water/sonication; GB1sp: Water/sonication/proteolysis; GB2s: NaOH/sonication; GB2sp: NaOH/sonication/proteolysis. The yield (g) increased in the following order GB2sp>GB1sp>GB1p>GB2s>GB1s>GB1. However, the amount of SP extracted increased in different way GB2sp>GB1p>GB1>GB1sp>GB1s>GB2s. Infrared and electrophoresis analysis showed that all conditions extracted the same SP. In addition, monosaccharide composition showed that ultrasound promotes the extraction of other polysaccharides than SP. In the prothrombin time (PT) test, which evaluates the extrinsic coagulation pathway, none of the samples showed anticoagulant activity. While in the activated partial thromboplastin time (aPTT) test, which evaluates the intrinsic coagulation pathway, all samples showed anticoagulant activity, except GB2s. The aPTT activity decreased in the order of GB1sp>GB2sp>GB1p>GB1>GB1s>GB2s. Total capacity antioxidant (TCA) of the SP was also affected by condition extraction, since GB2s and GB1 showed lower activity in comparison to the other conditions. In conclusion, the conditions of SP extraction influence their biological activities and chemical composition. The data showed NaOH/sonication/proteolysis was the best condition to extract anticoagulant and antioxidant SPs from Gracilaria birdiae.

Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.

Novos adsorventes para aplicação na remoção de enxofre de combustíveis

Currently the market requires increasingly pure oil derivatives and, with that, comes the need for new methods for obtaining those products that are more efficient and economically viable. Considering the removal of sulfur from diesel, most refineries uses catalytic hydrogenation process, the hydrodesulfurization. These processes needs high energy content and high cost of production and has low efficiency in removing sulfur at low concentrations (below 500 ppm). The adsorption presents itself as an efficient and economically viable alternative in relation to the techniques currently used. With that, the main purpose of this work is to develop and optimize the obtaining of new adsorbents based on diatomite, modified with two non ionic surfactants microemulsions, adding efficiency to the material, to its application on removal of sulfur present in commercial diesel. Analyses were undertaken of scanning electron microscopy (SEM), x-ray diffraction (XRD), x-ray fluorescence (XRF), thermogravimetry (TG) and N2 adsorption (BET) for characterization of new materials obtained. The variables used for diatomite modification were: microemulsion points for each surfactant (RNX 95 and UNTL 90), microemulsion aqueous phase through the use or non-use of salts (CaCl2 and BaCl2), the contact time during the modification and the contact form. The study of adsorption capacity of materials obtained was performed using a statistical modeling to evaluate the influence of salt concentration in the aqueous phase (20 ppm to 1500 ppm), finite bath temperature (25 to 60° C) and the concentration of sulphur in diesel. It was observed that the temperature and the concentration of sulphur (300 to 1100 ppm) were the most significant parameters, in which increasing their values increase the ability of modified clay to adsorb the sulphur in diesel fuel. Adsorption capacity increased from 0.43 to mg/g 1.34 mg/g with microemulsion point optimization and with the addition of salts.

Tratamento de cascalho de perfuração utilizando sistemas microemulsionados

The oil industry is one of the activities that generates more waste to the environment. The drill cuttings is a waste generated in large quantities in the drilling process and that may cause environmental damage such as soil contamination and consequently the contamination of groundwater if disposed of without prior treatment. Arises the need to develop scientific activities and research ways to adapt these wastes the current environmental standards. In the case of solid wastes, the NBR 10004: 2004 of the Brazilian Association of Technical Standards (ABNT) classifies them into class I waste (hazardous) and class II (not dangerous), which determines which wastes may or may not be discarded in the environment without causing environmental impact. This study presents a novel alternative for treating drill cuttings, where this waste was classified as class I (Abreu & Souza, 2005), mainly by removing the n-paraffin present in it, since this arises when using drilling fluids base oil. Using microemulsion systems promotes the removal of this contaminant drill cuttings samples from wells located in Alto do Rodrigues - RN. Initially, we determined the concentration of paraffin using infrared method in samples were extracted with ultrasound, we obtained a paraffin concentration in the range from 36.59 to 43.52 g of paraffin per kilogram of cuttings. Used two microemulsion systems containing two nonionic surfactants from different classes, one is an alcohol ethoxylated (UNTL-90) and the other an nonylphenol ethoxylated (RNX 110). The results indicated that the system UNTL-90 surfactant has better efficiency than the system with RNX 110. The study of the influence of contact time at the extraction showed that for times greater than 25 minutes has a tendency to increase the percentage extraction with increasing contact time. It was also observed that the extraction is fast because at 1 minute contact has 22.7% extraction. The reuse of the microemulsion system without removing the paraffin extracted in previous steps, showed reduction of 29.32 in percentage of extraction by comparing the first and third extraction, but by comparing the first and second extractions reduction is 8.5 in percentage extraction, so the systems reuse optimization can be an option for economically viable removing paraffin from cuttings. The extraction with shaking is more effective in the treatment of cuttings, reaching the extraction percentage of 87.04%, that is, obtaining a drill cuttings with 0.551% paraffin. Using the percentage of paraffin employed in non-aqueous drilling fluids and fluid maximum limit on cuttings for disposal established by the Environmental Protection Agency of the United States (US EPA), one arrives at the conclusion that the level of paraffin on gravel cannot exceed 3.93%. Conclude that the amount of paraffin in the treated cuttings with the microemulsion system with shaking is below the established by US EPA, showing that the system used was efficient in removing the paraffin from the drill cuttings.

Nanopartículas catiônicas de poli (ácido lático) para liberação modificada de peptídios da peçonha do escorpião Tityus serrulatus

Reported accidents involving the poisoning scorpions are still frequent in Brazil, mainly caused by Tityus serrulatus, known as yellow scorpion. Although antivenom sera are produced routinely by various government laboratories, the effectiveness of its use depends on how quickly treatment is initiated and efficiency in the production of antibodies by the immunized animals. In this study, the development of cationic polymeric nanoparticles of poly(lactic acid) aimed to create a modified delivery system for peptides and proteins of T. serrulatus venom, able to enhance the production of serum antibodies against the scorpion toxins. The cationic nanoparticles were obtained by a low energy nanoprecipitation, after study of the parameters’ variations effects over the physicochemical properties of the particles. The surface functionalization of the nanoparticles with the hyperbranched polyethyleneimine was proved by zeta potential analysis and enabled the adsorption by electrostatic interaction of different types of proteins. The protein loading efficiency of 40-80 % to bovine serum albumin (BSA) and 100 % to scorpion venom peptides evaluated by spectrophotometry and polyacrylamide gel electrophoresis confirmed the success of the selected parameters established for obtainment of nanoparticles, produced with size between 100 to 250 nm. The atomic force microscopy analysis and in vitro release showed that the spherical nanoparticles provided a sustained release profile of proteins by diffusion mechanism, demonstrating the potential for application of the nanoparticles in vivo.

Nanopartículas catiônicas de poli (ácido lático) para liberação modificada de peptídios da peçonha do escorpião Tityus serrulatus

Reported accidents involving the poisoning scorpions are still frequent in Brazil, mainly caused by Tityus serrulatus, known as yellow scorpion. Although antivenom sera are produced routinely by various government laboratories, the effectiveness of its use depends on how quickly treatment is initiated and efficiency in the production of antibodies by the immunized animals. In this study, the development of cationic polymeric nanoparticles of poly(lactic acid) aimed to create a modified delivery system for peptides and proteins of T. serrulatus venom, able to enhance the production of serum antibodies against the scorpion toxins. The cationic nanoparticles were obtained by a low energy nanoprecipitation, after study of the parameters’ variations effects over the physicochemical properties of the particles. The surface functionalization of the nanoparticles with the hyperbranched polyethyleneimine was proved by zeta potential analysis and enabled the adsorption by electrostatic interaction of different types of proteins. The protein loading efficiency of 40-80 % to bovine serum albumin (BSA) and 100 % to scorpion venom peptides evaluated by spectrophotometry and polyacrylamide gel electrophoresis confirmed the success of the selected parameters established for obtainment of nanoparticles, produced with size between 100 to 250 nm. The atomic force microscopy analysis and in vitro release showed that the spherical nanoparticles provided a sustained release profile of proteins by diffusion mechanism, demonstrating the potential for application of the nanoparticles in vivo.

Estudo da influência de sistemas microemulsionados na molhabilidade de arenitos e na recuperação avançada de petróleo

Sandstone-type reservoir rocks are commonly responsible for oil accumulation. The wettability is an important parameter for the physical properties of the container, since it interferes in characteristics such as relative permeability to the aqueous phase, residual oil distribution in the reservoir, operating characteristics with waterflood and recovery of crude oil. This study applied different types of microemulsion systems - MES - in sandstone reservoirs and evaluated their influences on wettability and residual oil recovery. For this purpose, four microemulsion were prepared by changing the nature of ionic surfactants (ionic and nonionic). Microemulsions could then be characterized by surface tension analysis, density, particle diameter and viscosity in the temperature range 30° C to 70° C. The studied oil was described as light and the sandstone rock was derived from the Botucatu formation. The study of the influence of microemulsion systems on sandstone wettability was performed by contact angle measurements using as parameters the rock treatment time with the MES and the time after the brine surface contact by checking the angle variation behavior. In the study results, the rock was initially wettable to oil and had its wettability changed to mixed wettability after treatment with MES, obtaining preference for water. Regarding rock-MES contact time, it was observed that the rock wettability changed more when the contact time between the surface and the microemulsion systems was longer. It was also noted only a significant reduction for the first 5 minutes of interaction between the treated surface and brine. The synthesized anionic surfactant, commercial cationic, commercial anionic and commercial nonionic microemulsion systems presented the best results, respectively. With regard to enhanced oil recovery performance, all systems showed a significant percentage of recovered oil, with the anionic systems presenting the best results. A percentage of 80% recovery was reached, confirming the wettability study results, which pointed the influence of this property on the interaction of fluids and reservoir rock, and the ability of microemulsion systems to perform enhanced oil recovery in sandstone reservoirs.

Estudo da influência de sistemas microemulsionados na molhabilidade de arenitos e na recuperação avançada de petróleo

Sandstone-type reservoir rocks are commonly responsible for oil accumulation. The wettability is an important parameter for the physical properties of the container, since it interferes in characteristics such as relative permeability to the aqueous phase, residual oil distribution in the reservoir, operating characteristics with waterflood and recovery of crude oil. This study applied different types of microemulsion systems - MES - in sandstone reservoirs and evaluated their influences on wettability and residual oil recovery. For this purpose, four microemulsion were prepared by changing the nature of ionic surfactants (ionic and nonionic). Microemulsions could then be characterized by surface tension analysis, density, particle diameter and viscosity in the temperature range 30° C to 70° C. The studied oil was described as light and the sandstone rock was derived from the Botucatu formation. The study of the influence of microemulsion systems on sandstone wettability was performed by contact angle measurements using as parameters the rock treatment time with the MES and the time after the brine surface contact by checking the angle variation behavior. In the study results, the rock was initially wettable to oil and had its wettability changed to mixed wettability after treatment with MES, obtaining preference for water. Regarding rock-MES contact time, it was observed that the rock wettability changed more when the contact time between the surface and the microemulsion systems was longer. It was also noted only a significant reduction for the first 5 minutes of interaction between the treated surface and brine. The synthesized anionic surfactant, commercial cationic, commercial anionic and commercial nonionic microemulsion systems presented the best results, respectively. With regard to enhanced oil recovery performance, all systems showed a significant percentage of recovered oil, with the anionic systems presenting the best results. A percentage of 80% recovery was reached, confirming the wettability study results, which pointed the influence of this property on the interaction of fluids and reservoir rock, and the ability of microemulsion systems to perform enhanced oil recovery in sandstone reservoirs.

El teorema de Riemann-Roch y el morfismo de Gysin en geometría aritmética

Le th eor eme de Riemann-Roch originale a rme que pour tout morphisme propre f : Y ! X entre vari et es quasi-projectifs lisses sur un corps, et tout el ement a 2 K0(Y ) du groupe de Grothendieck des br es vectoriels on a ch(f!(a)) = f {u100000}Td(Tf ) ch(a) (cf. [BS58]). Ici ch est le caract ere de Chern, Td(Tf ) est la classe de Todd du br e tangent relative et f et f! sont les images directes de l'anneau de Chow et K0 respectivement. Apr es, Baum, Fulton et MacPherson ont d emontr e en [BFM75] le th eor eme de Riemann-Roch pour des morphismes localement intersection compl ete entre des sch emas alg ebriques (sch emas s epar es et localement de type ni sur un corps) projectifs et singuli eres. En [FG83] Fulton et Gillet ont d emontr e le th eor eme sans hypoth eses projectifs. L'extension a la th eorie K sup erieure pour des sch emas r eguli eres sur une base fut d emontr e par Gillet en [Gil81]. Le th eor eme de Riemann-Roch qu'il prouve est pour des morphismes projectifs entre des sch emas lisses et quasi-projectifs. Donc, dans le cas des sch emas sur un corps, le r esultat de Gillet n'inclus pas le th eor eme de [BFM75]. La plus grande g en eralisation du th eor eme de Riemann-Roch que je connais est [D eg14] et [HS15], o u D eglise et Holmstrom-Scholbach obtiennent ind ependamment le th eor eme de Riemann- Roch pour la K-th eorie sup erieure et les morphismes projectifs lic entre sch emas r eguli eres sur une base noetherienne de dimension nie... NOTA 520 8 El teorema de Riemann-Roch original de Grothendieck a rma que para todo mor smo propio f : Y ! X, entre variedades irreducibles quasiproyectivas lisas sobre un cuerpo, y todo elemento a 2 K0(Y ) del grupo de Grothendieck de brados vectoriales se satisface la relaci on ch(f!(a)) = f {u100000}Td(Tf ) ch(a) (cf. [BS58]). Recu erdese que ch denota el car acter de Chern, Td(Tf ) la clase de Todd del brado tangente relativo y f y f! las im agenes directas en el anillo de Chow y K0 respectivamente. M as tarde Baum, Fulton MacPherson probaron en [BFM75] el teorema de Riemann-Roch para mor smos localmente intersecci on completa entre esquemas algebraicos (es decir, esquemas separados localmente de tipo nito sobre cuerpo) proyectivos singulares. En [FG83] Fulton y Gillet probaron el teorema sin hip otesis proyectivas. La notable extensi on a la teor a K superior para esquemas regulares sobre una base fue probada por Gillet en [Gil81]. El teorema de Riemann-Roch all probado es para mor smos proyectivos entre esquemas lisos quasiproyectivos. Sin embargo, obs ervese que en el caso de esquemas sobre cuerpo el resultado de Gillet no recupera el teorema de [BFM75]. La mayor generalizaci on del teorema de Riemann-Roch que yo conozco es [D eg14] y [HS15] donde D eglise y Holmstrom-Scholbach obtuvieron independientemente el teorema de Riemann-Roch para teor a K superior y mor smos proyectivos lic entre esquemas regulares sobre una base noetheriana nito dimensional...

Efeito da sinvastatina na sepse abdominal de ratos diabéticos

Analisar se o pré-tratamento com sinvastatina em modelo experimental de sepse abdominal é benéfico em ratos diabéticos. Métodos: Cinquenta e seis ratos Wistar foram aleatoriamente distribuídos em: grupo não diabético (n-28) e grupo diabetes induzido por estreptozotocina (n=28). Sepse abdominal por ligadura e punção do ceco foi induzida em 14 ratos diabéticos e em 14 não diabéticos. Os demais 28 animais foram alocados em grupo sham. Os grupos de ratos com sepse e os sham (cada com sete animais) foram tratados com microemulsão oral de simvastatina (20 mg kg-1 day-1) e solução salina 0,9%, respectivamente. Sangue periférico foi usado para dosagem de TNFa, IL-1b, IL-6, proteína C reativa, procalcitonina, contagem de leucócitos e neutrófilos em todos os animais. A análise estatística foi realizada pela ANOVA e teste de Tukey, com p<0,05. Resultados: A sinvastatina reduziu a mortalidade nos ratos diabéticos. Os valores séricos de TNF-a, IL-1b, IL-6, proteína C reativa, procalcitonina, leucócitos e neutrófilos mostraram-se mais baixos nos ratos diabéticos e não diabéticos com sepse, tratados com sinvastatina, do que nos tratados com solução salina. Conclusão: A sinvastatina teve efeito antiinflamatório, que pode ter resultado em proteção contra a sepse em ratos diabéticos

Produção enzimática de biodiesel a partir de resíduos agro-industriais usando a lipase imobilizada de origem microbiana

Trabalho Final de Mestrado para obtenção do grau de Mestre em Engenharia Química e Biológica

Efeito da sinvastatina na sepse abdominal de ratos diabéticos

Analisar se o pré-tratamento com sinvastatina em modelo experimental de sepse abdominal é benéfico em ratos diabéticos. Métodos: Cinquenta e seis ratos Wistar foram aleatoriamente distribuídos em: grupo não diabético (n-28) e grupo diabetes induzido por estreptozotocina (n=28). Sepse abdominal por ligadura e punção do ceco foi induzida em 14 ratos diabéticos e em 14 não diabéticos. Os demais 28 animais foram alocados em grupo sham. Os grupos de ratos com sepse e os sham (cada com sete animais) foram tratados com microemulsão oral de simvastatina (20 mg kg-1 day-1) e solução salina 0,9%, respectivamente. Sangue periférico foi usado para dosagem de TNFa, IL-1b, IL-6, proteína C reativa, procalcitonina, contagem de leucócitos e neutrófilos em todos os animais. A análise estatística foi realizada pela ANOVA e teste de Tukey, com p<0,05. Resultados: A sinvastatina reduziu a mortalidade nos ratos diabéticos. Os valores séricos de TNF-a, IL-1b, IL-6, proteína C reativa, procalcitonina, leucócitos e neutrófilos mostraram-se mais baixos nos ratos diabéticos e não diabéticos com sepse, tratados com sinvastatina, do que nos tratados com solução salina. Conclusão: A sinvastatina teve efeito antiinflamatório, que pode ter resultado em proteção contra a sepse em ratos diabéticos

(E)-2-[2-(2-Aminofenil)vinil]-1-metilquinolin-4(1H)-ona como precursor de novos compostos heterociclicos

Esta dissertação reporta a síntese de novos derivados de 4-quinolonas com potencial atividade biológica e está dividida em 3 capítulos. No primeiro capítulo é feita uma breve introdução aos compostos do tipo 4quinolona, azepina e indol, focando a nomenclatura, atividade biológica e métodos de síntese mais comuns deste tipo de compostos, e é apresentada a nomenclatura dos compostos sintetizados ao longo deste trabalho. No segundo capítulo são descritas as metodologias desenvolvidas para obtenção dos compostos pretendidos. Foram sintetizados novos derivados de 4-quinolonas via reações de N-metilação seguida de ciclização in situ da (E)-N(2-acetilfenil)-3-(2-nitrofenil)acrilamida, via reações de redução da 1-metil-2-[2(2-nitrofenil)vinil]quinolin-4(1H)-ona e reações de halogenação da 1-metil-2-[2(2-nitrofenil)vinil]quinolin-4(1H)-ona e da 2-[2-(2-aminofenil)vinil]-1metilquinolin-4(1H)-ona. Posteriormente, fizeram-se estudos de reatividade da 1-metil-2-[2-(2-nitrofenil)vinil]quinolin-4(1H)-ona e da 2-[2-(2-aminofenil)vinil]-3bromo-1-metilquinolin-4(1H)-ona. Na reação de redução in situ seguida de ciclização intramolecular da 1-metil-2-[2-(2-nitrofenil)vinil]quinolin-4(1H)-ona obteve-se a 2-(1H-indol-2-il)-1-metilquinolin-4(1H)-ona. Partindo da 2-[2-(2aminofenil)vinil]-3-bromo-1-metilquinolin-4(1H)-ona via reações de BuchwaldHartwig obteve-se a 11-metil-5H-benzo[6,7]azepino[3,2-b]quinolin-6(11H)-ona. Novas N-[2-(2-(3-bromo-1-metil-4-oxo-1,4-di-hidroquinolin-2il)vinil)fenil]alquilamidas foram obtidas via reações de acilação da 2-[2-(2aminofenil)vinil]-3-bromo-1-metilquinolin-4(1H)-ona em piridina seca usando diferentes cloretos de acilo. Numa tentativa de ciclização intramolecular da N[2-(2-(3-bromo-1-metil-4-oxo-1,4-di-hidroquinolin-2-il)vinil)fenil]-hexanamida via reação de Ullmann intramolecular foi obtida a 2-(1-hexanoil-1H-indol-2-il)-1metilquinolin-4(1H)-ona. Após a descrição detalhada das metodologias de síntese são apresentadas as principais conclusões deste trabalho e perspectivas futuras. Por último, no terceiro capítulo, são apresentados os procedimentos experimentais usados para obtenção dos compostos sintetizados e os dados relativos à sua caracterização estrutural, que foi sendo discutida ao longo do segundo capítulo. Os compostos sintetizados foram caracterizados por espetroscopia de ressonância magnética nuclear monodimensional (1H e 13C) e bidimensional (HSQC, HMBC) e por espetrometria de massa e sempre que possível por espetrometria de massa de alta resolução.

Uma Lectina D-lactose específica da esponja marinha Cinachyrella apion: purificação, caracterização e interação com Leishmania chagasi

Four different sponge species were screened using Ouchterlony agarose gel and immunodiffusion tests to identify cross-reactivity with the polyclonal antibody IgG anti-deglicosilated CvL, a lectin from Cliona varians. Crude extract from the sponge Cinachyrella apion showed cross-reactivity and also a strong haemmaglutinating activity towards human erythrocytes of all ABO groups. Thus, it was submitted to acetone fractionation, IgG anti-deglicosilated CvL Sepharose affinity chromatography, and Fast Protein Liquid Chromatography (FPLC-AKTA) gel filtration on a Superose 6 10 300 column to purify a novel lectin. C. apion lectin (CaL) agglutinated all types of human erythrocytes with preference for papainized type A and O erythrocytes. The haemagglutinating activity is independent of Ca2+, Mg2+ and Mn2+ ions, and it was strongly inhibited by the disaccharide D-lactose, up to a minimum concentration of 6.25 mM. CaL molecular mass determined by FPLC-AKTA gel filtration on a Superose 12 10 300 column and SDS gel electrophoresis was approximately 124 kDa, consisting of eight subunits of 15.5 kDa, assembled by hydrophobic interactions. The lectin was relatively heat- and pH-stable. Leishmania chagasi romastigotes were agglutinated by CaL, indicating that lactose receptors could be presented in this parasite stage. These findings are indicative of the physiological defense roles of CaL and its possible use in the antibiosis of pathogenic protozoa