The aim of this study was to develop and characterize poly-ε-caprolactone (PCL) and poly(D,L-lactic-co-glycolic)-acid (PLGA) microparticles containing coencapsulated trans-dehydrocrotonin (t-DCTN) and t-DCTN:hydroxypropyl-β-cyclodextrin inclusion complex (t-DCTN:HP-β-CD), with t-DCTN loaded at concentrations ranging from 11.25 to 45.00 mg. A preformulation study was carried out using a 24-1 fractional factorial design. Microparticles were prepared using the double w/o/w emulsion-solvent evaporation method. The coencapsulated t-DCTN:HP-β-CD-loaded PLGA microparticles (t-DCTN/t-DCTN:HP-β-CD/PLGA-MPs) presented a smaller particle size (9.6 ± 0.1 µm) and higher drug loading (13.93 ± 0.05%, corresponding to 90.1 ± 0.3% of encapsulation efficiency, EE) and t-DCTN-loaded PLGA microparticles (t-DCTN/PLGA-MPs) presented particle size of 37.0 ± 0.2 µm and drug loading of 10.12 ± 0.01% (EE of 71.2 ± 0.1%). The coencapsulation of t-DCTN and t-DCTN:HP-β-CD into PLGA microparticles increased drug loading (50%) and improved the drug controlled release (k2 = 0.0475 and De = 0.0475 × 10-11 cm2 s-1). Taking into account these findings, new oral formulation of PLGA microparticles containing coencapsulated t-DCTN and t-DCTN:HP-β-CD are available as biocompatible drug delivery systems for further pharmacological purposes.

Com o objetivo de estudar comparativamente o preparo intestinal para colonoscopia, 55 pacientes foram distribuídos aleatoriamente em grupos submetidos a preparo com polietilenoglicol (PEG) e solução de manitol. A qualidade do preparo do cólon no grupo que utilizou o PEG foi considerada excelente em 12 pacientes (44,4%), bom em 15 (55,6%) e ruim em nenhum caso, enquanto que naqueles indivíduos preparados com manitol a 20% a qualidade foi, respectivamente, de oito (28,6%), 12 (42,9%) e oito (28,6%) indivíduos, sendo a diferença estatisticamente significante (p=0,010). Não houve diferença estatística entre os grupos quando comparamos o grau de satisfação dos pacientes, ou a quantidade de líquido no cólon durante o exame. Conclui-se que a qualidade do preparo intestinal com PEG para colonoscopia é superior ao manitol.

With the aim of studying comparatively intestinal prepare for colonoscopy, 55 patients were randomly distributed into two groups that used polyethylene glycol (PEG) and mannitol solution. The quality of bowel prepare in the group that used PEG was considered excellent in 12 patients (44,4%), good in 15 (55,6%) and bad in no cases, while in those prepared with manitol the quality of intestine preparation was, respectively, eight (28,6%), 12 (42,9%) and eight (28,6%) patients. The difference was considered statistically significant (p=0,010). There wasn't any statistical difference between the groups when we compared the satisfaction degree of the patients or the amount of liquid in the colon during the colonoscopy. We can conclude that the quality of bowel preparation for colonoscopy with PEG is superior to manitol.

As atividades antiinflamatórias de oito compostos 4-amino-2,6-diarilpirimidina-5-carbonitrilas foram sujeitas a uma análise QSAR baseada nos resultados de cálculos de estrutura eletrônica B3LYP/6-31G(d,p) e AM1. Análise de Componentes Principais e regressões baseados nesses dados indicam que compostos potencialmente mais ativos teriam menores valores de momentos de dipolo e de coeficientes de partição e também seriam afetados pelos valores de cargas dos átomos de carbono através dos quais os dois anéis aromáticos estão ligados ao anel pirimidínico. Duas novas moléculas foram previstas serem, ao menos, tão ativas como aquelas com as maiores atividades usadas no estágio de construção do modelo. Uma delas, tendo o grupo metoxila conectado a um dos anéis aromáticos, foi prevista ter um valor de atividade antiinflamatória de 52,3%. Essa molécula foi sintetizada e sua atividade experimental foi determinada em 52,8%, em concordância com a previsão teórica AM1. Esse valor é 5% maior que o maior valor usado para a modelagem.

The experimental anti-inflammatory activities of eight 4-amino-2,6-diarylpyrimidine-5-carbonitriles were subjected to a QSAR analysis based on results from B3LYP/6-31G(d,p) and AM1 electronic structure calculations. Principal component analyses and regressions based on these data indicate that potentially more active compounds should have low dipole moment and partition coefficient values and also be affected by the values of the charges of the carbon atoms through which the two aromatic rings are bonded to the pyrimidinic ring. Two new molecules were predicted to be at least as active as those with the highest activities used in the model building stage. One of them, having a methoxy group attached to one of the aromatic rings, was predicted to have an anti-inflammatory activity value of 52.3%. This molecule was synthesized and its experimental activity was found to be 52.8%, in agreement with the AM1 theoretical prediction. This value is 5% higher than the largest value used for modeling.

Calibration transfer has received considerable attention in the recent literature. Several standardization methods have been proposed for transferring calibration models between equipments. The goal of this paper is to present a general revision of calibration transfer techniques. Basic concepts will be reviewed, as well as the main advantages and drawbacks of each technique. A case study based on a set of 80 NIR spectra of maize samples recorded on two different instruments is used to illustrate the main calibration transfer techniques (direct standardization, piecewise direct standardization, orthogonal signal correction and robust variable selection).

Hydrological samples were collected on the continental shelf of the Amazon river to determine particulate organic and inorganic matter, dissolved organic phosphorus (DOP), phosphate, total particulate phosphorus (TPP), chlorophyll a, temperature, salinity, pH, water transparency, dissolved oxygen (DO) and saturation rate. The objective was to study the forms of DOP, phosphate and TPP. In the euphotic layer, the fluvial discharge from the Amazon river favored the distribution of phosphate, TPP and DOP. In the aphotic layer, the phosphate concentration increased due to the decomposition of DOP and TPP. This increase is due to the absence of photosynthetic processes.

A desidratação osmótica é um processo que pode ser aplicado a frutos, para aumentar sua vida útil e, conseqüentemente, reduzir o percentual de perdas. Na aplicação deste processo em jenipapo, foi observada uma elevada incorporação de sólidos solúveis, considerada desvantajosa por reduzir a similaridade entre o produto e o fruto "in natura". Neste trabalho, foram empregados revestimentos comestíveis à base de alginato e pectina de baixa metoxilação, com o objetivo de diminuir a transferência de massa, cuja eficácia foi avaliada em jenipapos adquiridos nos supermercados da Região metropolitana do Recife, nas condições em que são comercializados. A pesquisa foi desenvolvida em duas etapas. A primeira, por meio de planejamento fatorial fracionário 2(3-1), com o objetivo de estudar a influência das coberturas, constituída por três tratamentos: A (frutos sem revestimento); B (frutos cobertos com alginato); e C (frutos cobertos com pectina. A segunda, por planejamento fatorial 2³, para determinar a influência das variáveis independentes, temperatura, tipo de cobertura e geometria sobre a perda de umidade, ganho de solutos, variação de peso e taxa de DEI (Dehydration Efficiency Index). Os resultados obtidos na 1ª etapa evidenciaram que: as coberturas foram eficientes na redução da incorporação de solutos, bem como no aumento de perda de umidade; os maiores DEI, em ambas as coberturas, foram obtidos a 50 °Brix, sendo o máximo a 30 °C e geometria representada por um quarto de fruta. Na 2ª etapa, foram confirmados maior influência da geometria sobre a perda de umidade e o ganho de solutos e das coberturas sobre a variação de peso e perda de umidade. Foi constatado que a temperatura exerce decisiva influência sobre as demais variáveis, com exceção dos DEI. Os resultados permitiram concluir que os menores ganhos de solutos, associados a uma satisfatória perda de umidade, foram obtidos com cobertura de alginato, geometria representada por um quarto de fruta, a 50 °Brix, independente das temperaturas, permitindo fixá-las em 50 °C.

Osmotic dehydration is a process that can be applied to fruit to increase their shelf life and hence reduce loss percentage. In the application of this process in jenipapo, a high incorporation of soluble solids was observed, considered disadvantageous because of the reduction of the similarity between the product and the fruit "in natura". In this work, low metoxilation alginate and pectin based edible coating were used to reduce this mass transfer. The effectiveness of these polysaccharides was evaluated in Jenipapos, purchased in supermarkets in the metropolitan area of the city of Recife, in the conditions in which they are sold. The research was developed in two stages: the first by means of a factorial design 2(3-1), consisting of three treatments: A (fruits without coating); B (fruits with alginate coating); and C (fruits with pectin coating) in order to study the influence of the coatings; in the second stage a factorial design 2³ was used in order to determine the influence of independent variables: temperature, coating type and geometry over moisture loss, solutes uptake, weight variation and rate of DEI (Dehydration Efficiency Index). The results obtained in the first stage showed that: the coatings were efficient in the reduction of solutes uptake as well as in the moisture loss increase, the higher DEI in both coatings were obtained at 50 °Brix, the highest DEI at 30 °C and the geometry was represented by the fruit cut in fourths. In the second stage a higher influence of the geometry over the moisture loss and the solute uptake as well as the coatings over the weight variation and moisture loss were confirmed. It was observed that the temperature exerts decisive influence over the other variables with the exception of the DEI. The results showed that the lower solutes uptake associated with a satisfactory moisture loss were obtained with alginate coating and the geometry was represented by the fruit cut in fourths, at 50 °Brix, regardless of the temperatures, allowing to set it at 50 °C.

Microbiological processes were used for chitin and chitosan productions by Cunninghamella elegans (UCP 542) grown in a new economic culture medium. The assay was carried out to evaluate the growth of C. elegans using yam bean (Pachyrhizus erosus L. Urban) medium, in different times of growth (24, 48, 72 and 96 hrs), incubated at 28ºC in an orbital shaker at 150 rpm. The lyophilized biomass was determined by gravimetry. The polysaccharides were extracted by alkali-acid treatment, and characterized by infrared spectroscopy, titration and viscosity. C. elegans grown in the yam bean medium and produced higher yields of biomass (24.3 g/ mL) in 96 hrs. The high level was chitosan (66 mg/g), and chitin (440 mg/g) were produced at 48 and 72 hrs of growth, respectively. The polysaccharides showed degree of deacetilation and viscosimetric molecular weight as: 6.2% and 3.25 x10(4) g/mol for chitin, and 85% and 2.72 x 10(4) g/mol for chitosan, respectively. The results obtained suggest high biotechnological potential of yam bean as an economic source to produce chitin and chitosan by C. elegans. In addition, the new medium using yam bean for production of the chitin and chitosan may be used for many purposes to reduce the cost price of fermentation processes.

Chemometric activities in Brazil are described according to three phases: before the existence of microcomputers in the 1970s, through the initial stages of microcomputer use in the 1980s and during the years of extensive microcomputer applications of the ´90s and into this century. Pioneering activities in both the university and industry are emphasized. Active research areas in chemometrics are cited including experimental design, pattern recognition and classification, curve resolution for complex systems and multivariate calibration. New trends in chemometrics, especially higher order methods for treating data, are emphasized.

O processo de desidratação osmótica foi aplicado ao Jenipapo (Genipa americana L.), para reduzir as perdas pós-colheita, diversificar o seu aproveitamento industrial e obter um produto com boas características organolépticas e boa estabilidade microbiológica. Os frutos foram adquiridos na feira livre de Afogados, na região metropolitana do Recife, nas condições em que são comercializados, subdivididos em cubos e submetidos a diversas condições de processamento, segundo planejamento fatorial 2³ de modo a determinar a influência das variáveis independentes: temperatura, tipo de açúcar e concentração do agente osmótico sobre a perda de umidade, ganho de açúcar e redução de peso. O processo foi complementado por secagem em estufa, com ventilação forçada a 60ºC±5ºC, por 3h±10', seguida do acondicionamento do produto em embalagem de polietileno e armazenamento à temperatura ambiente (28ºC±3ºC), por 90 dias. Os resultados demonstraram que: os produtos obtidos apresentaram significativa incorporação de sólidos; nenhuma das respostas foi influenciada pelo tipo de açúcar empregado, diferentemente da concentração do agente osmótico que além de refletir sobre todas elas, interagiu com a temperatura influindo sobre a perda de umidade; durante o armazenamento, os produtos apresentaram-se microbiologicamente estáveis, sem diferenças significativas, no que concerne às características organolépticas, embora os escores demonstrem uma preferência pelo produto obtido a partir de 60ºBrix, 60ºC e mistura de açúcar demerara e cristal. A elevada incorporação de sólidos ocorrida aponta para necessidade de proceder à otimização do produto com vista a sua redução.

The process of osmotic dehydration was applied in order to reduce the losses post-harvest, to diversify the industrial utilization of the jenipapo (Genipa americana L.), and to obtain a product with good organoleptic characteristic and good microbiological stability. The fruits were purchased in the street fair of Afogados, a district of Recife, in the conditions in which they are sold. They were cut in cubes and submitted to several conditions of processing, through a factorial design 2³ to determine the influence of independent variables: temperature, kind of sugar and osmotic agent concentration over moisture loss, sugar uptake and weight reduction. The process was complemented with drying in stove, with forced ventilation at 60ºC±5ºC for 3h±10', after which the products were packed in polyethylene packaging and stored at room temperature (28ºC±3ºC) for ninety days. The results demonstrated that: a significant solids uptake occurred; none of the obtained responses was influenced by the type of sugar used, whereas the osmotic agent concentration not only reflected on all of them it also interacted with the temperature influencing over moisture loss; during storage time, the products were microbiologically stable, without significant differences, in the organoleptic caracteristic, although the scores have showed a preference for the products obtained under the 60ºBrix, 60ºC and a blend of demerara and crystal sugar. The high solids uptake occurred points to a necessity to achieve the optimization of the products in order to reduce it.

This paper is a translation from IUPAC nomenclature document by K. Danzer and L. A. Currie (Pure Appl. Chem., 1998, 70(4), 993-1014). Its goal is to establish an uniform and meaningful approach to terminology (in Portuguese), notation, and formulation for calibation in analytical chemistry. In this first part, general fundamentals of calibration are presented, namely for both relationships of qualitative and quantitative variables (relations between variables characterizing certain types analytes of the measured function on the other hand and between variables characterizing the amount or concentration of the chemical species and the intensities of the measured signals, on the other hand). On this basis, the fundamentals of the common single component calibration (Univariate Calibration) which models the relationship y = f(x) between the signal intensities y and the amounts or concentrations x of the analyte under given conditions are represented. Additional papers will be prepared dealing with extensive relationships between several intensities and analyte contents, namely with multivariate calibrations and with optimization and experimental design.

Um planejamento fatorial de dois níveis foi empregado para analisar a influência da agitação, do tempo de contato, da quantidade de alga e do tipo de pré-tratamento sobre a remoção de metais pesados por algas Arribadas, num sistema em batelada contendo uma solução sintética simulando um efluente típico de fabricação de baterias. Amostras de 4 g de algas secas, moídas e peneiradas removeram 99% do chumbo de amostras de 100 mL do efluente sintético. Os percentuais máximos de remoção de zinco e ferro foram 37% e 80%, respectivamente. Como as algas arribadas são baratas, abundantes e de ocorrência natural, a remoção de chumbo através deste método pode ser vantajosa para aplicação industrial em larga escala.

A two-level factorial design was employed to analyze the influence of agitation, contact time, amount of algae and type of pretreatment on heavy metal removal by Arribadas algae, in a batch system consisting of a synthetic solution simulating a typical effluent from battery manufacturing processes. Dried, ground and sieved 4 g algae samples were able to remove 99 % lead from 100 mL samples of synthetic effluent. Maximum removals for zinc and iron were 37 % and 80 %, respectively. Lead removal using this method is potentially useful for large-scale industrial applications, because Arribadas algae are cheap, abundant, naturally occurring waste materials.

This review presents the evolution of simultaneous multicomponent analysis by absorption spectrophotometry in the ultraviolet and visual regions in terms of some qualitative and quantitative analysis techniques, otimization methods, as well as applications and modern trends.