Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 ºC. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, ¹H-NMR and 13C-NMR.

Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prep-HPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and ¹H-NMR spectra.

Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-β-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-β-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR).

Determination of sulfate in the wet-process of phosphoric acid by reverse flow injection

An improved method based on reverse flow injection is proposed for determining sulfate concentration in the wet-process of phosphoric acid (WPA). The effect of reagent composition, flow rate, temperature, acid concentration, length of the reaction coil, and linear response range on the flow system is discussed in detail. Optimal conditions are established for determining sulfate in the WPA samples. Baseline drift is avoided by a periodic washing step with EDTA in an alkaline medium. A linear response is observed within a range of 20 - 360 mg L-1, given by the equation A = 0.0020C (mg L-1) + 0.0300, R² = 0.9991. The detection limit of the proposed method for sulfate analysis is 3 mg L-1, and the relative standard deviation (n = 12) of sulfate absorbance peak is less than 1.60%. This method has a rate of up to 29 samples per hour, and the results compare well with those obtained with gravimetric method.

Utilization of retention chemicals in non-wood containing furnishes

The usage of the non-wood pulps in furnishes for various paper grades is the real alternative for substitution of wood fibres in the papermaking. This is especially important now, when the prices for wood are increasing and forest resources are depleting in many regions of our planet. However, there are several problems associated with utilization of such pulps. In terms of the papermaking process one of the main problems is the poor dewatering of the non-wood pulps. This problem can be partially solved by means of retention aids. In the literature part were described technological features of the non-wood pulps as the raw materials for paper production. Moreover, overviews of the retention chemicals and methods for retention measurement were done; special attention was paid to the mechanisms of retention and drainage. Finally, factors affecting on the drainage and retention of non-wood pulps were considered holistically. Particular emphasis was put on the possibility of enzyme treatment for drainage improvement. It was stated that retention aids can significantly improve dewatering of non-wood pulps. In the experimental part the goal was to investigate influence of various microparticle retention aids on the drainage, retention and formation of furnish containing wheat straw pulp, obtained by novel pulping process (Formico™Fib). The parallel test were performed with reference furnish containing only wood pulps. It was found that Bentonite-CPAM retention aid can significantly improve drainage and retention; however formation seems be suffer from such additives. It was stated that performance of the Silica-Starch retention aid significantly depends on the starch dosing sequence and wet-end conditions; this system have shown better formation than other tested retention aids. Silica-CPAM retention aid have provided comparable results in retention and drainage with Bentonite-CPAM, while Silica-starch did not improve dewatering and yielded in lowest filler retention among other aids. Ultimately, optimal dosages for the tested retention chemicals have been suggested.

The Effects of Some Furnish and Paper Structure Related Factors on Wet Web Tensile and Relaxation Characteristics

The objective of this thesis was to identify the effects of different factors on the tension and tension relaxation of wet paper web after high-speed straining. The study was motivated by the plausible connection between wet web mechanical properties and wet web runnability on paper machines shown by previous studies. The mechanical properties of wet paper were examined using a fast tensile test rig with a strain rate of 1000%/s. Most of the tests were carried out with laboratory handsheets, but samples from a pilot paper machine were also used. The tension relaxation of paper was evaluated as the tension remaining after 0.475 s of relaxation (residual tension). The tensile and relaxation properties of wet webs were found to be strongly dependent on the quality and amount of fines. With low fines content, the tensile strength and residual tension of wet paper was mainly determined by the mechanical interactions between fibres at their contact points. As the fines strengthen the mechanical interaction in the network, the fibre properties also become important. Fibre deformations caused by the mechanical treatment of pulp were shown to reduce the mechanical properties of both dry and wet paper. However, the effect was significantly higher for wet paper. An increase of filler content from 10% to 25% greatly reduced the tensile strength of dry paper, but did not significantly impair wet web tensile strength or residual tension. Increased filler content in wet web was shown to increase the dryness of the wet web after the press section, which partly compensates for the reduction of fibrous material in the web. It is also presumable that fillers increase entanglement friction between fibres, which is beneficial for wet web strength. Different contaminants present in white water during sheet formation resulted in lowered surface tension and increased dryness after wet pressing. The addition of different contaminants reduced the tensile strength of the dry paper. The reduction of dry paper tensile strength could not be explained by the reduced surface tension, but rather on the tendency of different contaminants to interfere with the inter-fibre bonding. Additionally, wet web strength was not affected by the changes in the surface tension of white water or possible changes in the hydrophilicity of fibres caused by the addition of different contaminants. The spraying of different polymers on wet paper before wet pressing had a significant effect on both dry and wet web tensile strength, whereas wet web elastic modulus and residual tension were basically not affected. We suggest that the increase of dry and wet paper strength could be affected by the molecular level interactions between these chemicals and fibres. The most significant increases in dry and wet paper strength were achieved with a dual application of anionic and cationic polymers. Furthermore, selectively adding papermaking chemicals to different fibre fractions (as opposed to adding chemicals to the whole pulp) improved the wet web mechanical properties and the drainage of the pulp suspension.

Carbohydrate intake in children - associations with dietary intakes, growth, serum lipids,and dental health. The STRIP Project

This study is part of the STRIP study, which is a long-term, randomized controlled trial, designed to decrease the exposure of children in the intervention group (n=540) to known risk factors of atherosclerosis. The main focus of the intervention was the quality of dietary fat. The control group (n=522) did not receive any individualized counselling. Food consumption was evaluated with food records, and blood samples were drawn and growth was measured regularly for all participating children from 13 months to 9 years. A subsample of 66 children participated in a dental health survey. The number of studies on children’s carbohydrate intake, especially fibre intake, is insufficient. The current international recommendations for fibre intake in children are based on average assumptions and data extrapolated from intakes in adults and intake recommendations for adults. Finnish nutrition recommendations lack strict recommendations for dietary fibre in children. Due to fibre’s high bulk volume, excessive dietary fibre is considered to decrease energy density and hence it may have an adverse effect on growth. If fats are reduced from the diet, the low-fat diet may become high in sucrose. Therefore, especially in the STRIP study, it is important to determine the use of fibre and sucrose in children and possible associations with growth and nutrition as well as dental health. The results of the present study indicate that a high fibre intake does not displace energy or disturb growth in children and that children with high fibre intake have better quality of diet than those with low fibre intake. Additionally, dietary fibre intake associated inversely with serum cholesterol concentration. Other carbohydrates also affected serum lipid levels as well, since total carbohydrates, sucrose, and fructose increased serum triglyceride concentration. Total carbohydrate intake reduced HDL cholesterol concentration only in children with apoE3 or apoE4 phenotype. Over the period from the 1970s to the 1990s the dental health of children in Finland has substantially improved despite an increase in sucrose intake. The improvement was thought to be due to improved dental hygiene and the use of fluorine. However, during the past twenty years improvement in dental health has stopped. The present study showed that high long-term sugar intake increases risk of caries in children. High intake of sugar had also negative effects on the diet of children, because it worsens dietary quality by displacing essential nutrients. Furthermore, the quality of dietary fat was worse in children with high sucrose intake. In this study the children’s high sucrose intake was not associated with overweight, but interestingly, it associated inversely with growth.

Komposiittien käyttö tämän päivän koneenrakennuksessa

Komposiitit ovat yhdistelmämateriaaleja, jotka koostuvat kahdesta tai useammasta eri materiaalista. Komposiitit ovat kiinnostavia tämän päivän koneenrakennukselle niiden korkean vahvuuden ja jäykkyyden suhteesta niiden kevyeeseen painoon nähden. Kuitulujitteisten komposiittien ja laminaattien valmistukseen on monia eri menetelmiä ja ne eroavat toisistaan lähinnä hartsin levittämistapojen sekä kuitujen asettelutapojen perusteella. Komposiittien työstäminen on vaikeaa, mikä johtuu niiden epähomogeenisesta ja anistrooppisesta laadusta ja komposiittien sisältävien lujitteiden korkeasta abrasiivisesta vaikutuksesta. Tavanomaisia työstömenetelmiä, kuten sorvausta, porausta ja jyrsimistä käytetään komposiittien työstämiseen. Kuitujen suuntaus komposiiteissa vaikuttaa paljon niiden työstämiseen. Ultraäänisen tärinän käyttäminen kuitulujitteisia komposiitteja sorvattaessa parantaa työstetyn kappaleen pinnanlaatua. Komposiittimateriaalien kiinnittäminen metalleihin eroaa selvästi muiden materiaalien kiinnittämisestä. Komposiittien yhdistämisen yhteydessä on otettava huomioon monia eri asioita, kiinnitysreikien valmistuksesta käytettäviin kiinnikkeisiin. Komposiittien kierrätys ja hävittäminen on tärkeä osa niiden elinkaarta, eikä niiden kierrätykseen ole tällä hetkellä hyviä ja kustannustehokkaita kierrätysmenetelmiä. Tällä hetkellä kierrättäminen tuleekin kalliimmaksi, kuin käytettyjen komposiittien vieminen kaatopaikalle.

Formando grupos no internato: critérios de escolha, satisfação e sofrimento psíquico

OBJETIVO: Descrever os critérios para formação de grupos no internato e a avaliação que os alunos fazem do relacionamento grupal, analisando as variáveis associadas. MÉTODO: Trata-se de um estudo transversal, que utilizou questionário autopreenchido, com perguntas sobre dados sociodemográficos, autoavaliação do desempenho escolar, critérios para formação e satisfação com grupo de internato. Sofrimento psíquico foi avaliado a partir do Self Report Questionnaire. Utilizou-se o teste do qui-quadrado e regressão logística para análise multivariada. RESULTADOS:A taxa de resposta no internato foi de mais de 90%. A maioria dos alunos utilizou critérios ligados à rede social (82,6%) e predominaram sujeitos satisfeitos com seu grupo (81,2%). Após análise multivariada, apenas autoavaliação do desempenho escolar "boa ou ótima" e critérios de escolha relacionados à rede de apoio se mantiveram associados à satisfação com o grupo. CONCLUSÕES: Apesar de ser um estágio da formação profissional, os alunos se escolheram por questões ligadas à rede social. Sendo uma profissão na qual o trabalho em equipe é inerente, deveriam ser criadas estratégias durante o curso médico para elaborar as dificuldades de relacionamento grupal entre alunos de Medicina.

Leiomioma do esôfago removido por videolaparoscopia

This report describes a leiomyoma of the inferior third section of the esophagus removed during laparoscopic cholecystectomy. The patient is a woman 55-years-age, carrying esophageal myoma of 40 mm in diameter wide, situated in the posterior wall of the lower esophagus. Indications for surgery were based mainly on the growth of the mass (6 mm when discovered 7 years previously, increased to 40 mm). Recently the patient returned suffering from pain, which could be attributed to his litiasic cholecystopaty. A small degree of low disphagia could also be observed. Radiologic imaging, direct endoscopic examination and endoscopic ultrasound showed that the mioma protruded on to the oesophagic lumen, discreetly diminishing there. A laparoscopic esophageal myomectomy was indicated at the same session of the laparoscopic cholecystectomy. Once the pneunoperitoneum was installed, five ports were placed as if for a hiatus hernia surgery. The cholecystectomy was uneventful. Next, an esophagoscopy was performed so as to determine the precise area covering the base of the tumour; at the right-lateral site. Longitudinal and circular fibres of the esophagus was severed over the lesion and the enucleation of the tumour was performed alternating the monopolar dissection, bipolar and hidrodisection. Control-endoscopy was carried out to verify mucosa integrity. Four suture points with poliglactine 3-0 string so as to close the musculature followed this. One suture was placed in for diminution of the size of the esophagean hiatus. Total time of intervention: two hours (30m for the cholecystectomy and one hour and thirty minutes for the myomectomy). Postoperative period: uneventful. Disappearance of the disphagia was observed. Radiologic transit control with water-soluble contrast at 4th post-operative day: good passage. Diagnosis from laboratory of pathology: conjunctive tumour formed by muscle non-striated cells: leiomyoma. The patient was re-examined on the two-month postoperative follow-up. General conditions were good and there were no complain of dysphagia. Neither there were any symptoms of gastro-esophageal reflux.

Geoprocessamento para identificar padrões do perfil de nascimentos na região do Vale do Paraíba

OBJETIVO: aplicar técnicas de geoprocessamento para a análise espacial do perfil de nascimentos por município. MÉTODOS: foi um estudo ecológico e exploratório com dados do Sistema de Informações de Saúde sobre nascidos vivos de 2004 e utilizando técnicas de geoprocessamento. Foram estimadas as autocorrelações espaciais das variáveis: parto cesáreo, escolaridade materna, baixo peso ao nascer, escore de Apgar de cinco minutos, prematuridade, número de consultas e mães adolescentes, além do mapa com o índice de desenvolvimento humano. Foi utilizada a estatística I de Moran para detecção de agregados de eventos no espaço, pelo programa TerraView 3.1.3 (desenvolvido pelo Instituto Nacional de Pesquisas Espaciais - INPE e de acesso público). Foram construídos mapas espaciais com estas variáveis e estimados os coeficientes de correlação de Pearson. RESULTADOS: os resultados mostraram que as proporções de nascidos vivos de mães com escolaridade acima de primeiro grau e de cesáreas, apresentaram padrão espacial visualmente identificável e autocorrelação espacial significativa. O baixo peso ao nascer, a prematuridade, o índice de Apgar, o número de consultas de pré-natal e o de mães adolescentes apresentaram padrão espacial aleatório, demonstrando que, nesta escala de análise, estes indicadores não discriminaram grupos de risco, apesar do seu inquestionável valor preditivo para morbimortalidade infantil em nível individual. Houve correlação positiva entre parto cesáreo e escolaridade, e entre parto cesáreo e índice de desenvolvimento humano e correlação negativa entre mães adolescentes e índice de desenvolvimento humano, com significância estatística (p<0,05). CONCLUSÕES: esta metodologia permitiu identificar aglomerados espaciais para as variáveis parto cesáreo e escolaridade materna, além de aprofundar o conhecimento sobre o perfil de nascimentos nos municípios, apresentando potencial no direcionamento de ações voltadas para áreas específicas.

Validação de questionário para avaliar a função sexual feminina após menopausa

OBJETIVO: elaborar e validar um questionário para medir os diferentes domínios da função sexual nas mulheres brasileiras pós-menopausa. MÉTODOS: participaram deste estudo 251 mulheres entre 2 e 15 anos após menopausa. Foi examinada a reprodutibilidade/confiabilidade do instrumento pelos coeficientes de correlação linear, intraclasse e concordância de Lin. A consistência interna foi examinada pelo coeficiente α de Cronbach. A verificação da face, conteúdo e construto seguiram diretrizes teóricas clássicas para validação de testes. RESULTADOS: foi gerado um instrumento inicial com 57 itens estruturados em nove domínios. Foram eliminados 14 (24,5%) questões por baixa correlação com a escala total ou pequeno poder de discriminação. A forma final com 43 itens demonstrou excelente reprodutibilidade (r=0,719; IC95%=0,690-0,750; pc=0,887; IC95%=0,850-0,930; p<0,001) e confiabilidade. A consistência interna da escala foi excelente (α de Cronbach 0,951) e cerca de 60% dos avaliadores confirmaram as validades de face e conteúdo. O exame da validade de construto mostrou adequação do instrumento (α=0,951). CONCLUSÕES: concluiu-se que o questionário proposto é adequado para examinar a função sexual feminina em mulheres pós-menopausa.

Loss of PTEN expression and AKT activation in HER2-positive breast carcinomas

PURPOSE: To examine the expression of AKT and PTEN in a series of HER2-positive primary invasive breast tumors using immunohistochemistry, and to associate these expression profiles with classic pathologic features such as tumor grade, hormone receptor expression, lymphatic vascular invasion, and proliferation.METHODS: A total of 104 HER2-positive breast carcinoma specimens were prepared in tissue microarrays blocks for immunohistochemical detection of PTEN and phosphorylated AKT (pAKT). Original histologic sections were reviewed to assess pathological features, including HER2 status and Ki-67 index values. The associations between categorical and numeric variables were identified using Pearson's chi-square test and the Mann-Whitney, respectively.RESULTS: Co-expression of pAKT and PTEN was presented in 59 (56.7%) cases. Reduced levels of PTEN expression were detected in 20 (19.2%) cases, and these 20 tumors had a lower Ki-67 index value. In contrast, tumors positive for pAKT expression [71 (68.3%)] were associated with a higher Ki-67 index value.CONCLUSION: A role for AKT in the proliferation of HER2-positive breast cancers was confirmed. However, immunohistochemical detection of PTEN expression did not correlate with an inhibition of cellular proliferation or control of AKT phosphorylation, suggesting other pathways in these mechanisms of control.

Citologia aspirativa no diagnóstico da linfadenite em ovinos

O presente estudo investigou o uso da cito-(73,0%), Arcanobacterium pyogenes (6,0%), Streptococlogia aspirativa com agulha fina no diagnóstico da lin-cus spp. β hemolítico (5,0%) e Escherichia coli (4,0%) fadenite em ovinos e a ocorrência de microrganismos foram os microrganismos mais frequentes nos animais nos linfonodos com lesões, com ênfase no isolamento de com linfadenite. Streptococcus spp. (21,0%) e Staphylo-Corynebacterium pseudotuberculosis. Foram utilizados coccus spp. (7,0%) foram as bactérias isoladas com 100 linfonodos de ovinos com aumento de volume su-maior frequência nos linfonodos sem lesões colhidos em gestivos de linfadenite e 100 linfonodos de ovinos sem abatedouro. A punção aspirativa com agulha fina perlesões, colhidos em abatedouro. C. pseudotuberculosis mitiu identificar microrganismos "corineformes" em 79 (79,0%) animais com linfadenite e, destes, 73 (73,0%) foram identificados como C. pseudotuberculosis. Nenhuma linhagem de C. pseudotuberculosis foi isolada dos linfonodos dos animais sem lesões. Concluiu-se que C. pseudotuberculosis foi o microrganismo mais freqüente nos ovinos com linfadenite, e que a citologia aspirativa pode ser utilizada como método de triagem no diagnóstico da linfadenite caseosa ovina