Bioanalytical method for the quantification of the monastrol derivative anticancer candidate lasom 65 in pre-clinical pharmacokinetic investigations

A simple HPLC/UV method was developed for the determination of the anticancer candidate LaSOM 65 in rat plasma. Samples were cleaned by protein precipitation with acetonitrile (recovery > 95%), after which they were subjected to chromatography under the isocratic elution of an acetonitrile:water (45:55, ν/ν) solution with detection at 303 nm. The method was linear (r² > 0.98) over the concentration range (0.05-2 µg mL-1) with intra- and inter-day precision ranging from 9.6% to 13.6% and 4.3% to 5.4%, respectively. The accuracy of the method ranged from 85% to 113.6%, and it showed sufficient sensitivity to determine pharmacokinetic parameters of LaSOM 65 after intravenous administration to Wistar rats.

Determinação do coeficiente de atividade na diluição infinita em sistemas etanol-água-sal por microextração em fase sólida-gc-fid

A new method using the headspace solid phase microextraction (HS-SPME) technique was used to evaluate the infinite dilute activity coefficient (γ1∞) in an alcohol/water/salt system. The studied systems were ethanol and water with NaCl and NH4Cl at salt concentrations of 5, 10, 15, and 30% m/v and temperatures of 303.15 and 313.15 K. The method was used to investigate the salt effect on vapor/liquid equilibrium in an ethanol/water system, yielding satisfactory results. The study focused on the rich side in ethanol. The data were compared with the literature infinite dilution data determined by other methods such as differential ebulliometry (EBUL), differential static cell equilibrium (STAT), and gas-liquid chromatography with no gas phase correction (GC). In this study, NaCl showed better separation rates than NH4Cl.

NANOPARTICLES OF TUNGSTEN AS LOW-COST MONOMETALLIC CATALYST FOR SELECTIVE HYDROGENATION OF 3-HEXYNE

Low-cost tungsten monometallic catalysts containing variable amounts of metal (4.5, 7.1 and 8.5%W) were prepared by impregnating alumina with ammonium metatungstate as an inexpensive precursor. The catalysts were characterized using ICP, XPS, XRD, TPR and hydrogen chemisorption. These techniques revealed mainly WO3-Al2O3 (W6+) species on the surface. The effects of the content of W nanoparticles and reaction temperature on activity and selectivity for the partial hydrogenation of 3-hexyne, a non-terminal alkyne, were assessed under moderate conditions of temperature and pressure. The monometallic catalysts prepared were found to be active and stereoselective for the production of (Z )-3-hexene, had the following order: 7.1WN/A > 8.5 WN/A ≥ 4.5 WN/A. Additionally, the performance of the synthesized xWN/A catalysts exhibited high sensitivity to temperature variation. In all cases, the maximum 3-hexyne total conversion and selectivity was achieved at 323 K. The performance of the catalysts was considered to be a consequence of two phenomena: a) the electronic effects, related to the high charge of W (+6), causing an intensive dipole moment in the hydrogen molecule (van der Waals forces) and leading to heterolytic bond rupture; the H+ and H- species generated approach a 3-hexyne adsorbate molecule and cause heterolytic rupture of the C≡C bond into C- = C+; and b) steric effects related to the high concentration of WO3 on 8.5WN/A that block the Al2O3 support. Catalyst deactivation was detected, starting at about 50 min of reaction time. Electrodeficient W6+ species are responsible for the formation of green oil at the surface level, blocking pores and active sites of the catalyst, particularly at low reaction temperatures (293 and 303 K). The resulting best catalyst, 7.1WN/A, has low fabrication cost and high selectivity for (Z )-3-hexene (94%) at 323 K. This selectivity is comparable to that of the classical and more expensive industrial Lindlar catalyst (5 wt% Pd). The alumina supported tungsten catalysts are low-cost potential replacements for the Lindlar industrial catalyst. These catalysts could also be used for preparing bimetallic W-Pd catalysts for selective hydrogenation of terminal and non-terminal alkynes.

Magnetic, thermal and spectral characterization of 2,6-dimethoxybenzoates of Co(II), Ni(II) and Cu(II)

The complexes of 2,6-dimethoxybenzoic acid anion with ions of Co(II), Ni(II), and Cu(II) have been synthesized as polycrystalline solids, and characterized by elemental analysis, spectroscopy, magnetic studies, and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have following colours: pink for Co(II), green for Ni(II), and blue for Cu(II) compounds. The carboxylate group binds as monodentate, and bidentate bridging and chelating ligands. On heating in air to 1173 K the complexes decompose in four, three or two steps. At first, they dehydrate in one or two steps to anhydrous salts, that next decompose to oxides of the respective metals. The solubility of the investigated dimethoxybenzoates in water at 293 K is of the order of 10-2 mol/dm3. Their magnetic moments were determined in the temperature range of 76-303 K. The results reveal the compounds of Co(II) and Ni(II) to be high-spin complexes and that of Cu(II) to form dimer.

Magnetic, thermal and spectral properties of Ni(II) 2,3- , 3,5- and 2,6-dimethoxybenzoates

Complexes of Ni(II) 2,3-, 3,5- and 2,6-dimethoxybenzoates have been synthesized, their physico-chemical properties have been compared and the influence of the position of -OCH3 substituent on their properties investigated. The analysed compounds are crystalline, hydrated salts with green colour. The carboxylate ions show a bidentate chelating or bridging coordination modes. The thermal stabilities of Ni(II) dimethoxybenzoates were investigated in air in the range of 293-1173 K. The complexes decompose in three steps, yelding the NiO as the final product of decomposition. Their solubilities in water at 293 K are in the order of 10-2-10-4 mol×dm-3. The magnetic susceptibilities for the analysed dimethoxybenzoates of Ni(II) were measured over the range of 76-303 K and the magnetic moments were calculated. The results reveal that the complexes are the high-spin ones and the ligands form the weak electrostatic field in the octahedral coordination sphere of the central Ni(II) ion. The various position -OCH3 groups in benzene ring cause the different steric, mesomeric and inductive effects on the electron density in benzene ring.

Magnetic, thermal and spectral behaviour of 3-chloro-2-nitrobenzoates of Co(II), Ni(II), and Cu(II)

Physico-chemical properties of 3-chloro-2-nitrobenzoates of Co(II), Ni(II) and Cu(II) were synthesized and studied. The complexes were obtained as mono- and dihydrates with a metal ion to ligand ratio of 1 : 2. All analysed 3-chloro-2-nitrobenzoates are polycrystalline compounds with colours depending on the central ions: pink for Co(II), green for Ni(II) and blue for Cu(II) complexes. Their thermal decomposition was studied in the range of 293 ­ 523 K, because it was found that on heating in air above 523 K 3-chloro-2-nitrobenzoates decompose explosively. Hydrated complexes lose crystallization water molecules in one step and anhydrous compounds are formed. The final products of their decomposition are the oxides of the respective transition metals. From the results it appears that during dehydration process no transformation of nitro group to nitrite takes place. The solubilities of analysed complexes in water at 293 K are of the order of 10-4 ­ 10-2 mol / dm³. The magnetic moment values of Co2+, Ni2+ and Cu2+ ions in 3-chloro-2-nitrobenzoates experimentally determined at 76 ­ 303 K change from 3.67µB to 4.61µB for Co(II) complex, from 2.15µB to 2.87µB for Ni(II) 3-chloro-2-nitrobenzoate and from 0.26µB to 1.39µB for Cu(II) complex. 3-Chloro-2-nitrobenzoates of Co(II) and Ni(II) follow the Curie-Weiss law. Complex of Cu(II) forms dimer.

Magnetic, thermal and spectral characterization of 2,4-dimethoxybenzoates of Mn(II), Co(II) and Cu(II)

2,4 - Dimethoxybenzoates of Mn(II), Co(II) and Cu(II) have been synthesized as hydrated or anyhydrous polycrystalline solids and characterized by elemental analysis, IR spectroscopy, magnetic studies and X-ray diffraction measurements. They possess the following colours: Mn(II) - white, Co(II) - pink and Cu(II) - blue. The carboxylate groups bind as monodentate, or a symmetrical bidentate bridging ligands and tridentate. The thermal stabilities were determined in air at 293-1173K. When heated the hydrated complexes dehydrate to from anhydous salts which are decomposed to the oxides of respective metals. The magnetic susceptibilites of the 2,4-dimethoxybenzoates were measured over the range 76-303 K and their magnetic moments were calculated. The results reveal the complexes of Mn(II), Co(II) to be high-spin complexes and that of Cu(II) to form dimer.

Synthesis and magnetic properties of heteronuclear 3d-4f compound

A novel heteronuclear 3d-4f compound having formula NdCu3L3·13H2O (where H3L = Schiff base derived from 5-bromosalicylaldehyde and glycylglycine and L³ = C11H8 N2O4Br) was obtained. It was characterized by elemental and thermal analyses and magnetic measurements. The Cu(II)-Nd(III) compound is stable up to 323 K. During dehydration process the water molecules are lost in two stages. The magnetic susceptibility data for this complex change with temperature according to the Curie-Weiss law with theta = -35 K. The magnetic moment values decrease from 5.00µB at 303 K to 4.38µB at 76 K.

Complexes of 3,4-dimethoxybenzoic acid anion with Cu(II), Co(II), La(III), and Nd(III)

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.

Synthesis, characterization and thermal behaviour of heavy trivalent lanthanide malonates

Solid-state Ln-L compounds, where Ln stands for heavy trivalent lanthanides (Tb-Lu) and L is malonate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, TG-FTIR system, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The dehydration of the compounds begins at 303 K and the anhydrous compounds are stable up to 548 K. The results also provided information concerning the ligand's denticity, thermal behaviour and identification of some gaseous products evolved during the thermal decomposition of these compounds.

Incidência de podridões do colmo, grãos ardidos e rendimento de grãos em híbridos de milho submetidos ao aumento na densidade de plantas

A adequada combinação entre a escolha da densidade de plantas e do híbrido é um dos fatores que contribuem para o aumento da produtividade do milho. O objetivo deste trabalho foi avaliar o efeito do incremento na densidade de plantas sobre a incidência de podridões do colmo, de grãos ardidos e o rendimento de grãos de dois híbridos de milho contrastantes quanto a tolerância ao adensamento. O experimento foi conduzido em Lages, SC, nas safras agrícolas 2002/03 e 2003/04, em área de semeadura direta e monocultura, sob sucessão de cobertura morta constituída de aveia preta+ervilhaca. Estudou-se a combinação de dois fatores: híbrido e densidades, utilizando-se o delineamento experimental de blocos casualizados com parcela sub-dividida. Na parcela principal avaliaram os híbridos: Speed (simples, tolerante ao adensamento) e AG 303 (duplo, intolerante ao adensamento). Nas sub-parcelas testaram-se cinco densidades de plantas: 25, 50, 75, 100 e 125 mil plantas ha-1. O aumento da densidade de plantas, proporcionou incremento linear na incidência das podridões do colmo e grãos ardidos para os dois híbridos e duas safras avaliadas. O fungo Colletotrichum graminicola foi o mais detectado em colmos doentes, seguido do Fusarium graminearum, F. verticillioides e Stenocarpella sp. Nos grãos ardidos, os fungos predominantes foram F. verticillioides, F. graminearum e Penicillium spp. O híbrido AG 303 demonstrou menor resposta no rendimento do que o híbrido Speed com o aumento da população de plantas. Não foi observada associação direta entre o maior rendimento de grãos do híbrido simples em estandes adensados e a menor incidência de doenças de colmo e de grãos ardidos.

Consumo de álcool e fumo entre os estudantes da Faculdade de Medicina da Universidade Federal de Uberlândia

É preocupante o crescimento do consumo de substâncias psicoativas entre a população, o que constitui um grave problema de saúde pública. Entre as substâncias psicoativas, o álcool e o tabaco merecem destaque, pois são drogas lícitas e socialmente aceitas. Este estudo buscou estabelecer a prevalência do uso de bebidas alcoólicas e cigarros entre estudantes da Faculdade de Medicina da Universidade Federal de Uberlândia (Famed/UFU), bem como caracterizar as situações propícias, a freqüência, a auto-avaliação sobre consumo e o tipo de bebida utilizado por esses estudantes. Os dados foram coletados de uma amostra de 303 acadêmicos matriculados na Famed/UFU, a partir de questionário anônimo. Constatou-se que 66,34% dos alunos entrevistados consomem bebidas alcoólicas. Há aumento de ingestão de bebidas no decorrer do curso, sendo que os homens consomem mais que as mulheres. Apenas 3,3% do total de estudantes são fumantes e 2% são ex-fumantes. Esses números sugerem que a consciência sobre os malefícios do cigarro é maior do que a existente sobre o consumo abusivo de bebidas alcoólicas, no qual um comportamento de risco é observado.

Identificação de conflito de uso da terra em áreas de preservação permanente no entorno do parque nacional do Caparaó, Estado de Minas Gerais

Este estudo teve como objetivos elaborar um mapa de uso da terra com base nas imagens do satélite IKONOS II, delimitar de maneira automática as áreas de preservação permanente e identificar a ocorrência de conflitos de usos, tendo como referência legal o Código florestal e a Resolução n.º 303 do CONAMA. A pesquisa foi desenvolvida na entorno do Parque Nacional do Caparaó, pertencente aos municípios de Alto Jequitibá, Alto Caparaó, Caparaó e Espera Feliz, todos situados no estado de Minas Gerais. Utilizando os recursos disponíveis no geoprocessamento, foi possível mapear 8 classes de uso da terra e delimitar as áreas de preservação permanente situadas em áreas com altitudes superior a 1.800 metros (8,42 ha), no terço superior dos morros (18,67 ha); encostas com declividade superior a 45 graus (92,96 ha); nascentes e suas respectivas áreas de contribuição (1.989,44 ha); margens dos cursos d´água com largura inferior a 10 metros (3.957,19 ha); e no terço superior das sub-bacias (6.031,54 ha), perfazendo um total de 12.098,22 ha (48,06%) da área total da bacia. A área de uso indevido correspondeu a 8.922,91 ha (73,75%), sendo as classes cafezal (5.183,43 ha) e pastagem (3.650,74 ha) as principais ocorrências nessas áreas. Apenas 2.160,69 ha (18,40%) das áreas de preservação permanente estão protegidas por vegetação nativa.

Mapeamento das áreas de preservação permanente e identificação dos conflitos de uso da terra na sub-bacia hidrográfica do Rio Camapuã/Brumado

O objetivo deste trabalho foi mapear e quantificar as áreas de preservação permanente (APPs) de acordo com a Resolução nº 303/02 do CONAMA para, então, com base no mapa de uso da terra e cobertura vegetal, identificar e quantificar os eventuais conflitos de uso da terra, com vistas a nortear o cumprimento da lei e promover o uso adequado dos recursos da sub-bacia hidrográfica do rio Camapuã/Brumado, MG. Utilizaram-se uma imagem digital do sensor ETM+/LANDSAT 7, bases cartográficas planialtimétricas do IBGE para a área de estudo, e os softwares Anudem 5.2, Erdas Imagine 9.2 e ArcGIS 9.3. As APPs ocuparam 63.095 ha, representando 57,0% da área total da sub-bacia (110.711,9 ha). Com relação às categorias de APPs, o terço superior da bacia, ao longo das linhas de cumeada, correspondeu a 52,6% dos 63.095 ha; as zonas de proteção às margens dos cursos d'água, a 31,4%; a proteção das nascentes, a 15,6%; e as encostas com declividade superior a 45° e o terço superior de morros totalizaram 0,4%. As áreas de terço superior da bacia, ao longo das linhas de cumeada, foram as mais desrespeitadas (55,9%), seguidas das margens de curso d'água (23,12%), proteção de nascentes (20,83%), encostas com declividade superior a 45° (0,3%) e terço superior de morros (0,1%). Foram identificados 21.939,3 ha de APPs sendo explorados por atividades agropecuárias, o que representa 34,8% do total de APPs. Entretanto, constatou-se que 30.734,3 ha dos 47.616,9 ha situados fora das áreas de APP, i.e., 64,5% das áreas legalmente passíveis de conversão de uso da terra, estavam cobertos por vegetação nativa. Encontraram-se sólidas evidências de que a falta de conhecimento a respeito da espacialização das APPs dentro da propriedade é a principal causa do descumprimento da lei. A delimitação e espacialização das APPs pelo geoprocessamento viabilizam a aplicação da legislação florestal, contribuindo notoriamente para minimizar os conflitos de uso da terra e evitar a degradação dos remanescentes florestais pela formação de corredores ecológicos naturais que mitiguem os efeitos deletérios da fragmentação de habitats.

Diagnóstico das áreas de preservação permanente na bacia hidrográfica do Rio Tijuco, Ituiutaba - MG, utilizando tecnologia SIG

O presente trabalho teve como objetivo elaborar o mapa de uso da terra e cobertura vegetal da bacia hidrográfica do Rio Tijuco, município de Ituiutaba - MG, com base nas imagens digitais obtidas do satélite CBERS 2, através de delimitação automática das áreas de preservação permanente, seguindo-se a identificação de ocorrência de conflito de uso, tendo como referência legal o Código Florestal Brasileiro (Lei nº. 4.771/1965) e a resolução nº 303/02, do Conselho Nacional do Meio Ambiente. Este artigo analisa, por meio de parâmetros quantitativos e uso do Sistema de Informação Geográfica, a manutenção de faixas de preservação permanente de larguras recomendadas pela legislação ao longo dos corpos d'água. Os resultados mostraram um déficit de áreas preservadas às margens dos rios de 2.334 ha, que não estão em conformidade com a legislação. A pastagem ocupa, indevidamente, 0,97% da área da bacia nas áreas de preservação permanente às margens dos rios, enquanto a agricultura ocupa 0,38%.