1000 resultados para nitrobenzoic acid
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An amperometric sensor was constructed, by using humic acids to immobilize Fe3+ ions on a carbon paste electrode (CPE-HA-Fe), and used for ascorbic acid (H2A) determination. The cyclic voltammogram of the electrode showed electrochemical response due to the Fe3+/Fe2+ couple at E1/2=+0.78 V vs SCE, using 0.5 mol L-1 KCl and 0.2 mol L-1 acetate/0.020 mol L-1 phosphate buffer, at pH = 5.4, as supporting electrolyte. When H2A is added to the electrolyte solution it is observed an oxidation process. The oxidation current, obtained by chronoamperommetry at +0.87 V vs SCE, is proportional to the concentration, represented by the equation I(µA) = 7.6286 [H2A] (mmol L-1) + 1.9583, r = 0.9996, for concentrations between 0.0 and 1.4 mmol L-1. The electrode showed high stability and was used for H2A determination in a natural orange juice.
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The stoichiometry of the polyanions formed by the action of nitric acid on sodium tungstate (< 0.01M) has been studied by means of electrometric techniques involving pH-potentiometric and conductometric titrations. The well defined inflections and breaks in the titration curves provide evidence for the existence of the polyanions, para-W12O41(10-) and meta-W12O39(6-) corresponding to the ratio of H+:WO4(2-) as 7:6 and 9:6 in the pH ranges 5.7-6.0 and 3.6-4.1, respectively. The interaction of lanthanum nitrate with sodium tungstate solutions, at specific pH levels 8.0, 5.9 and 4.0 was also studied by pH and conductometric titrations, in aqueous and alcoholic media, with each of the reagents alternatively used as titrant. The electrometric experiments provide definite evidence of the formation of normal-La2O3.3WO3, para-5La2O3.36WO3 and meta-La2O3.12WO3 tungstates in the vicinity of pH 6.3, 5.0 and 4.2, respectively. Analytical investigations on the precipitates formed confirm the results of the electrometric study.
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The inhibition of the corrosion of mild steel in 2M hydrochloric acid solutions by Pyridoxol hydrochloride (PXO) has been studied using weight loss and hydrogen evolution techniques. The inhibitor (PXO) exhibited highest inhibition efficiency of 71.93% at the highest inhibitor concentration of 1.0 x 10-2M investigated and a temperature of 303K from weight loss result. Also, inhibition was found to increase with increasing concentration of the inhibitor and decreasing temperature. A first order type of mechanism has been deduced from the kinetic treatment of the weight loss results and the process of inhibition attributed to physical adsorption. The results obtained from the two techniques show that pyridoxol hydrochloride could serve as an effective inhibitor of the corrosion of mild steel in HCl acid solution. The compound obeys the Langmuir adsorption isotherm equation.
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Physico-chemical properties of 3,4-dimethoxybenzoates of Co(II), Cu(II), La(III) and Nd(III) were studied. The complexes were obtained as hydrated or anhydrous polycrystalline solids with a metal ion-ligand mole ratio of 1 : 2 for divalent ions and of 1 : 3 in the case of trivalent cations. Their colours depend on the kind of central ion: pink for Co(II) complex, blue for Cu(II), white for La(III) and violet for Nd(III) complexes. The carboxylate groups in these compounds are monodentate, bidentate bridging or chelating and tridentate ligands. Their thermal decomposition was studied in the range of 293-1173 K. Hydrated complexes lose crystallization water molecules in one step and form anhydrous compounds, that next decompose to the oxides of respective metals. 3,4 - Dimethoxybenzoates of Co(II) is directly decomposed to the appropriate oxide and that of Nd(III) is also ultimately decomposed to its oxide but with the intemediate formation of Nd2O2CO3.. The magnetic moment values of 3,4-dimethoxybenzoates determined in the range of 76-303 K change from 4.22 µB to 4.61 µB for Co(II) complex , from 0.49 µB to 1.17 µB for Cu(II) complex , and from 2.69 µB to 3.15 µB for Nd(III) complex.
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Unprocessed native starches are structurally too weak and functionally too restricted for application in today's advanced food technologies. Processing is necessary to engender a range of functionality. Naturals or natives starches can be modified by using several methods physical, chemical, enzymatic or combined, according industrial purposes. In this work, native corn starch was hydrolyzed by hydrochloric acid solution and investigated by using thermoanalytical techniques (thermogravimetry - TG, differential thermal analysis - DTA and differential scanning calorimetry - DSC), as well as optical microscopy and X-ray diffractometry. After acid treatment at 30 and 50°C, a decrease of gelatinization enthalpy (ΔHgel) was verified. Optical microscopy and X-ray diffractometry allowed us to verify the granules contorn and rugosity typical of cereal starches.
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Propolis is a sticky, gummy, resinous substance collected by honeybees (Apis mellifera L.) from various plant sources, which has excellent medicinal properties. This paper describes the isolation and identification of triterpenoids and anacardic acid derivatives from Brazilian propolis and their antibacterial activity. Their structures were elucidated by ¹H and 13C NMR, including uni- and bidimensional techniques; in addition, comparisons were made with data from academic literature. These compounds were identified as: cardanols (1a + 1b), cardols (2a + 2b), monoene anacardic acid (3), a-amirine (4), b-amirine (5), cycloartenol (6), 24-methylene-cycloartenol (7) and lupeol (8). The determination of the position of the double bond after a reaction with Dimethyl disulfide (DMDS) is described for the phenol derivatives. The ethanolic extract was tested in vitro for antimicrobial activity by using the disc diffusion method and it showed significant results against Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa and Shigella spp.
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The 2-methoxycinnamylidenepyruvic acid (2-MeO-HCP) was synthesized and characterized for nuclear magnetic resonance (¹H and 13C NMR), mass spectrometry (MS), Infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The application of DSC for purity determination is well documented in literature and is used in the analysis of pure organic compounds. The molecular geometry and vibrational frequencies of 2-MeO-HCP have been calculated.
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In this work, a new mathematical equation correction approach for overcoming spectral and transport interferences was proposed. The proposal was applied to eliminate spectral interference caused by PO molecules at the 217.0005 nm Pb line, and the transport interference caused by variations in phosphoric acid concentrations. Correction may be necessary at 217.0005 nm to account for the contribution of PO, since Atotal217.0005 nm = A Pb217.0005 nm + A PO217.0005 nm. This may be easily done by measuring other PO wavelengths (e.g. 217.0458 nm) and calculating the relative contribution of PO absorbance (A PO) to the total absorbance (Atotal) at 217.0005 nm: A Pb217.0005 nm = Atotal217.0005 nm - A PO217.0005 nm = Atotal217.0005 nm - k (A PO217.0458 nm). The correction factor k is calculated from slopes of calibration curves built up for phosphorous (P) standard solutions measured at 217.0005 and 217.0458 nm, i.e. k = (slope217.0005 nm/slope217.0458 nm). For wavelength integrated absorbance of 3 pixels, sample aspiration rate of 5.0 ml min-1, analytical curves in the 0.1 - 1.0 mg L-1 Pb range with linearity better than 0.9990 were consistently obtained. Calibration curves for P at 217.0005 and 217.0458 nm with linearity better than 0.998 were obtained. Relative standard deviations (RSD) of measurements (n = 12) in the range of 1.4 - 4.3% and 2.0 - 6.0% without and with mathematical equation correction approach were obtained respectively. The limit of detection calculated to analytical line at 217.0005 nm was 10 µg L-1 Pb. Recoveries for Pb spikes were in the 97.5 - 100% and 105 - 230% intervals with and without mathematical equation correction approach, respectively.
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Thermal stability and thermal decomposition of succinic acid, sodium succinate and its compounds with Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) were investigated employing simultaneous thermogravimetry and differential thermal analysis (TG-DTA) in nitrogen and carbon dioxide atmospheres and TG-FTIR in nitrogen atmosphere. On heating, in both atmospheres the succinic acid melt and evaporate, while for the sodium succinate the thermal decomposition occurs with the formation of sodium carbonate. For the transition metal succinates the final residue up to 1180 ºC in N2 atmosphere was a mixture of metal and metal oxide in no simple stoichiometric relation, except for Zn compound, where the residue was a small quantity of carbonaceous residue. For the CO2 atmosphere the final residue up to 980 ºC was: MnO, Fe3O4, CoO, ZnO and mixtures of Ni, NiO and Cu, Cu2O.
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Växtoljor som utgör en förnybar naturresurs används som sådana eller i modifierade former i många industriella processer, som är av stor betydelse för vårt vardagliga liv. Växtoljor används i livsmedel, i kemiska och farmaceutiska produkter, i textilindustrin, för framställning av färgämnen och beläggningsmaterial samt som miljövänliga bränslekomponenter. Fetter och oljor hör till de äldsta kemiska komponenterna som utnyttjas av människan. De består huvudsakligen av glycerolestrar och fettsyror. Fetter och oljor har typiskt en kolkedja med kol-koldubbelbindningar samt karboxyl- och estergrupper, som kan genom hydrering eller dekarboxylering konverteras till nyttiga och miljövänliga produkter med hjälp av ädelmetallkatalysatorer. Aktivt kol (C) används som bärare på katalysatorerna. Väteaddition, d.v.s. hydrering av växtoljor har varit föremål för omfattande forskning i över hundra års tid. Hydreringen är en viktig process, för den tillämpas på produktion av fetter och margarin. Omättade fettsyror hydreras traditionellt på nickelbaserade heterogena katalysatorer. Samtidigt med en partiell hydrering av fettsyrorna och fettsyraestrarna som har två dubbelbindningar pågår också isomeringsreaktioner, vilka ger cis- och transisomerer av reaktantmolekylerna. Den största nackdelen med nickelkatalysatorerna är deras giftighet samt bildning av ohälsosamma transisomerer i reaktionsprodukterna. Dessutom deaktiveras nickelkatalysatorn snabbt p.g.a. att nickeltvålar bildas i reaktionsblandningen. Platinabaserade katalysatorer lider däremot inte av dessa begränsningar. Metaller i platinagruppen i det periodiska systemet studerades i detalj för att avslöja kinetiska effekter i hydreringen av cis-metyloleat. Palladium, rutenium, rhodium, platina och iridium användes som katalytiska metaller. Metallhalten på aktivkolbärare var 1 vikt-%. De olika platinametallerna undersöktes för att kartlägga konkurrerande hydrerings- och isomeringsrutter på metallerna. Det visade sig att metallerna i andra raden av det periodiska systemet (Ru, Rh, Pd) är aktivare i isomeringsprocesserna, medan metallerna i tredje raden (Ir, Pt) har en lägre aktivitet. Pd/C valdes bland platinametallerna, för att den är attraktiv ur ekonomisk synvinkel och den är mycket aktiv och selektiv, speciellt jämfört med nickel. Tyngdpunkten i arbetet var utvecklingen av en alternativ, palladiumbaserad hydreringsteknologi som skulle ersätta den traditionella teknologin som är baserad på användningen av nickelkatalysatorer. Palladiumbaserade katalysatorer kan återcirkuleras, de är aktivare och mera resistenta mot syror och de bildar mindre mängder av skadliga transisomerer. För att denna teknologi skall bli ekonomiskt hållbar och konkurrenskraftig, måste den basera sig på de bästa möjliga katalysatorerna, vilket innebär att en optimal kombination av hög aktivitet och selektivitet samt en lång livstid för katalysatorn krävs. Därför inkluderades teknologiska aspekter kraftigt i forskningen. Mycket arbete satsades på design av palladium på en mesoporös kolbärare och undersökning av korrelationerna mellan katalysatorns egenskaper och dess aktivitet i isomeriseringsreaktionerna och i hydreringen av kol-koldubbelbindningarna i reaktantmolekylen. Katalysatorerna karakteriserades med många fysikaliska och kemiska metoder (transmissionselektronmikroskopi (TEM), röntgendiffraktion (XRD), röntgenfotoelektronspektroskopi (XPS), temperaturprogrammerad reduktion (TPR), temperaturprogrammerad desorption (TPD) av kolmonoxid, kemisorption av kolmonoxid, fysisorption av kväve). Temperaturens, vätetryckets och katalysatorkoncentrationens inverkan på fettsyra- och isomersammansättningen hos de hydrerade oljorna bestämdes under kinetiska betingelser, i frånvaro av massöverföringseffekter. Syreavspjälkning genom fullständig dekarboxylering av karboxylgruppen i fettsyramolekylen är det hittills bästa sättet att framställa miljövänlig dieselolja, eftersom linjära paraffiner fås som reaktionsprodukter och en tillsats av dyr vätgas undviks. Deoxygeneringen undersöktes systematiskt på en Pd/C-katalysator (Sibunit) genom att använda mättade fettsyror C16-C20 och C22 som råvara. Produktmolekylen blev en dieselliknande kolvätemolekyl, med en kolatom färre än i utgångsmolekylen. Lika stora dekarboxyleringshastigheter observerades för rena, mättade fettsyror. En jämförelse av deoxygenereringshastigheterna för stearin-, olein- och linolsyra som råvara vid 300oC i närvaro av 1-volymprocent väte på mesoporös Pd/C (Sibunit) avslöjade att katalysatorns aktivitet och selektivitet ökade med en ökande mättningsgrad av reaktantmolekylen. Då stearinsyra användes som utgångsmolekyl, bestod huvudprodukterna av önskade C17-kolväten, medan mängden av aromatiska C17-komponenter ökade, då olein- och linolsyra användes som utgångsmolekyler. Katalysatordeaktiveringen var relativt påfallande vid deoxygeneringen av linolsyra så att endast 3% av fettsyrorna omsattes till produkter i 330 min. Deaktiveringen orsakades av aromatiska C17-komponenter samt av fettsyradimerer, som bildades via en Diels-Alderreaktion. Hydreringen av omättade fettsyror kan därför rekommenderas som ett primärt kemiskt steg i framställningen av miljövänliga dieselprodukter. Målet var också att öka förståelsen av palladiummetallernas roll i nanoskala, speciellt effekten av metallpartiklarna i katalytisk hydrering och deoxygenering. Pd/C-katalysatorer med lika stora halter av Pd syntetiserades och metallens dispersion på bärarmaterialet varierades systematiskt genom en kontrollerad uppväxt av palladiumnanopartiklar på aktiv kolbärare. Metalldispersionens effekt på hydrerings-hastigheten och cis-transförhållandet undersöktes i detalj. En optimal metalldispersion som gav den högsta dekarboxyleringshastigheten hittades. Massöverföringens inverkan på reaktionens hastighet studerades experimentellt och temperaturprogrammerad desorption av kolmonoxid från katalysatorytan undersöktes ingående. Hydrering av växtoljor genomfördes under satsvisa och kontinuerliga betingelser. Både finfördelat Pd/C och katalysatorgranulat användes i experimenten. Ett av målen med arbetet var uppskalningen av hydreringsprocesserna. Med tanke på stora produktionsvolymer var det logiskt att undersöka kontinuerliga hydrerings- och dekarboxyleringsteknologier. En kontinuerlig packad bäddreaktor studerades i laboratorieskala, vilket gav viktig information om katalysatorns långtidsstabilitet och deaktivering. Effekten av rena fettsyror och triglycerider som råvara samt metallpartikelstorleken och palladiumhalten studerades med hjälp av den kontinuerliga reaktorn. Produktionskapaciteten som erhölls med satsvis och kontinuerlig drift jämfördes. Dekarboxyleringen av stearinsyra undersöktes också i en kontinuerlig packad bädd. Omsättningsgraden blev 15% för en stabil katalysator.
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The overall purpose of this thesis was to increase the knowledge on the biogeochemistry of rural acid sulphate (AS) soil environments and urban forest ecosystems near small towns in Western Finland. In addition, the potential causal relationship between the distribution of AS soils and geographical occurence of multiple sclerosis (MS) disease was assessed based on a review of existing literature and data. Acid sulphate soils, which occupy an area of approximately 17–24 million hectare worldwide, are regarded as the nastiest soils in the world. Independent of the geographical locality of these soils, they pose a great threat to their surrounding environment if disturbed. The abundant metal-rich acid drainage from Finnish AS soils, which is a result of sulphide oxidation due to artificial farmland drainage, has significant but spatially and temporally variable ecotoxicological impacts on biodiversity and community structure of fish, benthic invertebrates and macrophytes. This has resulted in mass fish kills and even eradication of sensitive fish species in affected waters. Moreover, previous investigations demonstrated significantly enriched concentrations of Co, Ni, Mn and Al, metals which are abundantly mobilised in AS soils, in agricultural crops (timothy grass and oats) and approximately 50 times higher concentrations of Al in cow milk originating from AS soils in Western Finland. Nevertheless, the results presented here demonstrate, in general, relatively moderate metal concentrations in oats and cabbage grown on AS soils in Western Finland, although some of the studied fields showed anomalous values of metals (e.g. Co and Ni) in both the soil and target plants (especially oats), similar to that of the previous investigations. The results indicated that the concentrations of Co, Ni, Mn and Zn in oats and Co and Zn in cabbage were governed by soil geochemistry as these metals were correlated with corresponding concentrations extracted from the soil by NH4Ac-EDTA and NH4Ac, respectively. The concentrations of Cu and Fe in oats and cabbage were uncorrelated to that of the easily soluble concentrations in the soils, suggesting that biological processes (e.g. plant-root processes) overshadow geochemical variation. The concentrations of K and Mg in cabbage, which showed a low spread and were strongly correlated to the NH4Ac extractable contents in the soil, were governed by both the bioavailable fractions in the topsoil and plant-uptake mechanisms. The plant´s ability to regulate its uptake of Ca and P (e.g. through root exudates) seemed to be more important than the influence of soil geochemistry. The distribution of P, K, Ca, Mg, Mn and S within humus, moss and needles in and around small towns was to a high degree controlled by biological cycling, which was indicated by the low correlation coefficients for P, K, Ca, Mg and S between humus and moss, and the low spread of these nutrients in moss and needles. The concentration variations of elements in till are mainly due to natural processes (e.g. intrusions, weathering, mineralogical variations in the bedrock). There was a strong spatial pattern for B in humus, moss and needles, which was suggested to be associated with anthropogenic emissions from nearby town centres. Geogenic dust affected the spatial distribution of Fe and Cr in moss, while natural processes governed the Fe anomaly found in the needles. The spatial accumulation patterns of Zn, Cd, Cu, Ni and Pb in humus and moss were strong and diverse, and related to current industry, the former steel industry, coal combustion, and natural geochemical processes. An intriguing Cu anomaly was found in moss. Since it was located close to a main railway line and because the railway line´s electric cables are made of Cu, it was suggested that the reason for the Cu anomaly is corrosion of these cables. In Western Finland, where AS soils are particularly abundant and enrich the metal concentrations of stream waters, cow milk and to some extent crops, an environmental risk assessment would be motivated to elucidate if the metal dispersion affect human health. Within this context, a topic of concern is the distribution of multiple sclerosis as high MS prevalence rates are found in the main area of AS soils. Regionally, the AS soil type in the Seinäjoki area has been demonstrated to be very severe in terms of metal leaching, this area also shows one of the highest MS rates reported worldwide. On a local scale, these severe AS soil types coincide well with the corresponding MS clustering along the Kyrönjoki River in Seinäjoki. There are reasons to suspect that these spatial correlations are causal, as multiple sclerosis has been suggested to result from a combination of genetic and environmental factors.
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Epileptic seizures are harmful to the developing brain. During epileptic seizures, overactivation of glutamate receptors (GluR) leads to neuronal degeneration, defined as excitotoxicity. The hippocampus is especially vulnerable to excitotoxic neuronal death, but its mechanism has remained incompletely known in the developing brain. Recently, signs of activation of inflammatory processes after epileptic seizures have been detected in the hippocampus. The purpose of this thesis was to study the inflammatory reaction and death mechanisms in excitoxic neurodegeneration induced by the glutamate analogue kainic acid (KA) in the developing hippocampus. Organotypic hippocampal slice cultures (OHCs), prepared from 6-7-day-old rats (P6-7) and treated with KA, served as an in vitro model. KA-induced status epilepticus in P9 and P21 rats was used as an in vivo model. The results showed that the pyramidal cell layers of the hippocampus were the most susceptible to irreversible and age-specific neurodegeneration, which occurred in the juvenile (P21), but not in the immature (P9), rat hippocampus. The primary death mechanism was necrosis as there were no significant changes in the expression of selected apoptosis markers and morphological cellular features of necrosis were found. Inflammatory response was similarly age-dependent after KA treatment as a rapid, fulminant and wide response was detected in the juvenile, but not in the immature, rat brain. An anti-inflammatory drug treatment, given before KA, was not neuroprotective in OHCs, possibly because of the timing of the treatment. In summary, the results suggest that KA induces an age-dependent inflammatory response and necrotic neurodegeneration, which may cause disturbances in hippocampal connectivity and promote epileptogenesis.
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The objective of this work was to evaluate the feasibility of vegetative propagation through cutting technique of seven tree species with strong occurrence in the riparian forest of the Lower São Francisco River in Sergipe State, under different concentrations of indolbutiric acid at 0, 2500, and 5000 mg.L-1, for potentialization of its use in soil bioengineering technique. It was used a complete random block design with three replicates, and a total of twenty-one treatments. The evaluation period was 120 days for each species, and the data collection was made in intervals of fifteen days, in a total of eight evaluations for each species. The evaluated parameters were: Survival Rate, callus formation, and Root Dry matter Weight. Among the studied species, Schinus terebinthifolius Raddi presented the best results related to cutting technique mainly under the indolbutiric acid concentration of 2500 mg.L-1.
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Batch chromatography is a widely used separation technique in a variety of fields meeting difficult separations. Several technologies for improving the performance of chromatography have been studied, including mixed-recycle steady state recycling (MR-SSR) chromatography. Design of MR-SSR has been commonly limited on 100 % purity constraint cases and empirical work. In this study a predictive design method was used to optimize feed pulse size and design a number of experimental MR-SSR separations for a solution of 20 % sulfuric acid and 100 g/L glucose. The design was under target product fraction purities of 98.7 % for H2SO4 and 95 % for glucose. The experiments indicate a maximum of 59 % increase in sulfuric acid productivity and 82 % increase for glucose when compared to corresponding batch separation. Eluent consumption was lowered by approximately 50 % using recycling chromatography. Within this study the target purities and yields set in design were not completely met, and further optimization of the process is deemed necessary.
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OBJECTIVE: To evaluate the effect of preoperative supplementation of omega-3 fatty acids on the healing of colonic anastomoses in malnourished rats receiving paclitaxel. METHODS: we studied 160 male Wistar rats, divided in two groups: one subjected to malnutrition by pair feeding (M) for four weeks, and another that received food ad libitum (W). In the fourth week, the groups were further divided into two subgroups that received omega-3 or olive oil by gavage. The animals were submitted to colonic transection and end-to-end anastomosis. After the operation, each of the four groups was divided into two subgroups that received intraperitoneal isovolumetric solutions of saline or paclitaxel. RESULTS: mortality was 26.8% higher in the group of animals that received paclitaxel (p = 0.003). The complete rupture strength was greater in well-nourished-oil Paclitaxel group (WOP) compared with the the malnourished-oil Paclitaxel one (MOP). The collagen maturation index was higher in well-nourished-oil saline group (WOS) in relation to the malnutrition-oil-saline group (MOS), lower in malnourished-oil-saline group (MOS) in relation to malnourished-ômega3-saline one (M3S) and lower in the well-nourished-omega3-saline group (W3S) compared with the malnourished-omega3-saline (M3S). The blood vessel count was higher in the malnourished-oil-saline group (MOS) than in the malnourished-oil-paclitaxel group (MOP) and lower in the malnourished-oil-saline group (MOS) in relation to the malnourished-omega3-paclitaxel group (M3P). CONCLUSION: supplementation with omega-3 fatty acids was associated with a significant increase in the production of mature collagen in malnourished animals, with a reversal of the harmful effects caused by malnutrition associated with the use of paclitaxel on the rupture strength, and with a stimulus to neoangiogenesis in the group receiving paclitaxel.