Validation of a stability indicating capillary electrophoresis method for the determination of darunavir in tablets and comparison with the of infrared absorption spectroscopic method

Darunavir (DRV) is a protease inhibitor used in the treatment of HIV infection, which constitutes a keystone in the therapy of patients infected with this virus. There is no monograph described in official compendia. The literature provides few methods of analysis for the determination of DRV in pharmaceuticals which include TLC, IR, UPLC, HPLC, HPLC-MS, HPLC-MS/MS, but there are no reports of the use of capillary electrophoresis (CE) for the determination of this drug. Thus, this research proposed the development and validation of a CE method for the determination of DRV in tablets. The method was completely validated according to the International Conference on Harmonization guidelines, showing linearity, selectivity, precision, accuracy and robustness. The migration was achieved in less than 1 minute using fused-silica uncoated capillary with an id of 50 μm and total length of 21 cm and voltage of +20 kV. The sample injection was performed in the hydrodynamic mode. The method was linear over the concentration range of 50-200 μg mL-1 with correlation coefficient 0.9998 and limits of detection and quantification of 7.29 and 22.09 μg mL-1, respectively. The drug was subjected to acid, base, oxidation and photolysis degradation. Degradation products were found interfering with the assay of DRV, therefore the method can be regarded as stability indicating. The validated method is useful and appropriate for the routine quality control of DRV in tablets.

Efeito do jejum sobre o desempenho zootécnico, crescimento e degradação muscular e alterações hepáticas de juvenis de pacu Piaractus mesopotamicus

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Comparative analysis of the cranial osteology and evolutionary traits of micrastur gilvicollis, micrastur ruficollis and micrastur semitorquatus (aves: falconiformes)

The cranial osteology of Micrastur gilvicollis (Vieillot, 1817), Micrastur ruficollis (Vieillot, 1817) and Micrastur semitorquatus (Vieillot, 1817) is comparatively and meticulously described to characterize each of the species and to determine which traits the species have in common and which are distinct. These traits will be used a posteriori for phylogenetic analysis. Our results indicate that M. gilvicollis and M. ruficollis are closely related, as they share a large number of traits, including a lacrimal bone with a distal portion that is approximately half as long as the proximal portion and a parasphenoid rostrum that covers 50% of the distance between the occipital condyle and pterygoid. Similarly, M. gilvicollis and M. semitorquatus both have a partially fused craniofacial flexion zone. In both M. ruficollis and M. semitorquatus, the symphyseal region of the mandible is 1/5 the total length of the mandible. The diagnostic traits for each of these species are as follows: a) in M. gilvicollis, the interorbital distance is 1/3 the length of the parietal, and the zygomatic process stretches 1/5 of the distance from the orbital arch to the jugal arch; b) in M. ruficollis, the interorbital distance is 2/5 of the length of the parietal and the zygomatic process extends 1/4 of the distance from the orbital arch to the jugal arch; and c) in M. semitorquatus, the interorbital distance is 3/7 the length of the parietal and the distal portion of the lacrimal is 1/3 the length of the proximal portion. Among the three species, M. gilvicolis and M. ruficollis share the most traits, which leads us to infer that these species are more closely related to one another than they are to M. semitorquatus. Phylogenetic analysis performed a posteriori may confirm the relationship between these three species.

Osteologia craniana comparada de Caracara cheriway (Jacquin, 1784) e Caracara plancus (Miller, 1777) (AVES: FALCONIDAE)

The Caracara genus (Aves: Falconidae) is composed by species C. cheriway, ("Crested Caracara"), and C. plancus (Southern Caracara). This study aimed to describe in detail and compared the cranial osteology of C. cheriway and C. plancus, identifying osteological cranial characters for a future systematic work. The two common characters of Caracara species are: the projection of rostro parasphenoid reaches 50% of the distance from the occipital condyle to the pterygoid; the upper maxilla has about 4/9 of the total length of theskull, the symphysial portion of mandible occupies about 1/7 of its total length, the proximal portion of lacrimal bone ends in a rounded shape and has about 1/4 of the width of the distal portion. The unique characters of C. cheriway are: the interorbital width is about 1/2 of the parietal region, shows a frontal bone prominence; presence of lacrimal process of frontal bone; the proximal portion of the lacrimal bone reaches 1/5 of the distance from the orbital arc to the jugal bone; the distance between the distal portions of two lacrimal bones reach 5/6 of the parietal width, the ratio between the interorbital diameter and parietal region ranges from 2 times; the zygomatic process occupies about 40% of the distance between its origin in the skull and jugal bone. The unique characters of C. plancus are: the interorbital width is approximately 4/7 of the parietal width; show a rostral medial concavity; the proximal portion of the lacrimal bone is about 1/4 of the width of the distal; the proximal portion of the lacrimal bone reaches 1/7 of the distance from the orbital arc to the jugal bone; the distance between the distal portions of two lacrimal bones reaches 6/7 of the width parietal one; the ratio between the interorbital diameter and parietal region varies 1, 75 times, the zygomatic process occupies about 35% of the distance between its origin in the skull and jugal bone.

Construção e validação de um túnel de vento para ensaios de estimativa da deriva em pulverizações agrícolas

The aim of this study was to build and validate a low cost reduced-scale wind tunnel for drift evaluation on pesticide application technology. The work was carried out at the NEMPA - Núcleo de Ensaio de Máquinas e Pneus Agroflorestais (NEMPA), FCA/UNESP, Departamento de Engenharia Rural, Botucatu/SP, Brazil. The wind tunnel main characteristics were an open circuit and a closed working section with a fan blowing air into the tunnel. Screens were fitted downstream after the fan in order to stabilize the air flow on the working section. The tunnel was built with 3.0 mm eucalyptus hardboard, with a total length of 4.8 m and a squared section of 0.56 m. The air flow was provided by a 180 W axial fan. The system was adjusted and calibrated to provide a laminar and stable flow at 2.0 m s-1. Validation studies were carried out by using a Teejet XR 8003 flat fan nozzle at 200 kPa (medium droplets) to apply a spray solutions containing water plus a food dye (Blue FDC) at 0,6% m v-1 mixed with two adjuvants: a polymer based anti drift formulation at 0,06% m v-1 and a sodium lauryl ether sulfate based surfactant at 0,2% v v-1. After a 10-second application the drift was collected on nylon strips transversally fixed along the tunnel at different distances from the nozzle and different high from the bottom part of the tunnel. Drift deposits were evaluated by spectrophotometry. The wind tunnel had low levels of turbulence and high repeatability of the data, which means that the flow was uniform and able to be used for carrying out measures to estimate drift. The validation results showed that the tunnel was effective to enable comparative drift measurements on the spray solution used in this work making possible the evaluation of drift risk potential under those spray technologies. The use of an adjuvant based on a polymer reduced the amount of drift from the nozzle compared to the surfactant.

Análise da efetividade de polimerização, adaptação marginal e interna de restaurações Classe II de resinas compostas de inserção em bloco utilizando diferentes matrizes

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Variações sazonais dos níveis plasmáticos do esteroide sexual 17β-estradiol (e2) em fêmeas de matrinxã (brycon amazonicus)

Pós-graduação em Ciência e Tecnologia Animal - FEIS

Long-Term Adult Population Fluctuations and Distribution of the Spot, Leiostomus xanthurus, in Mississippi

Adult specimens of the spot. Leiostomus xanthurus, were collected from bayou, Mississippi Sound, and barrier island locations along the Gulf Coast of Mississippi from November 1982 to July 1989. 7he mean total length of all spot sampled in comparable gill net sets was 219 mm (± 14 standard deviation, n=4,338). Ninety-five percent of the spot were collected in the island and sound areas, where the salinity was higher than in the bayous. Catch per unit effort was high at island and sound stations in spring and autumn, with relatively few fish caught during the winter spawning season and summer. The relatively high frequency of spot observed at the island stations in the autumn was probably influenced by spawning migrations, and the high spring values may represent a combination of two abundant year classes. The two greatest yearly collections, in 1983 and 1986, may have been influenced by sampling conditions or by environmental conditions favorable to survival either during those years or earlier when those fish were postlarvae. The smallest yearly catch occurred in 1985 and may have reflected the harsh weather conditions that year.

Spatial modelling and prediction on river networks: up model, down model or hybrid?

Preservation of rivers and water resources is crucial in most environmental policies and many efforts are made to assess water quality. Environmental monitoring of large river networks are based on measurement stations. Compared to the total length of river networks, their number is often limited and there is a need to extend environmental variables that are measured locally to the whole river network. The objective of this paper is to propose several relevant geostatistical models for river modeling. These models use river distance and are based on two contrasting assumptions about dependency along a river network. Inference using maximum likelihood, model selection criterion and prediction by kriging are then developed. We illustrate our approach on two variables that differ by their distributional and spatial characteristics: summer water temperature and nitrate concentration. The data come from 141 to 187 monitoring stations in a network on a large river located in the Northeast of France that is more than 5000 km long and includes Meuse and Moselle basins. We first evaluated different spatial models and then gave prediction maps and error variance maps for the whole stream network.

Biometric relationships of the spotted lobster, Panulirus echinatus, from Tamandare coastal reefs, Pernambuco State, Brazil

Biometric relationships were recorded for 2431 male and female Panulirus echinatus sampled at Tamandare coastal reefs, Pernambuco, Brazil. The following body measurements were taken: carapace length and width, abdomen length and width, total length, third and fifth pereiopod length, cephalothorax-abdomen and total weight. Twelve relationships were studied to compare the biometric characteristics Of males and females. Eleven of them showed difference between the sexes. Comparing sexes with the same carapace length, males have a heavier cephalothorax and longer third and fifth pereiopods than females, whereas females are longer, wider, and have a heavier abdomen than males. For genders with the same total length, males are heavier and have a longer carapace than females, while females have a larger abdomen. For genders with the same abdomen length, males have a heavier abdomen than females. The relationships TWg/TL and A Wg/AL showed positive allometric growth for the males. All other relationships involving weight, presented negative allometric growth for both sexes.

Allometry and population structure of Nicolea uspiana (Polychaeta: Terebellidae)

The relative growth and population structure of the terebellid Nicolea uspiana were investigated in the intertidal zone of a rocky shore on the south-east coast of Brazil, from May 2006 to May 2007. Eight hundred and forty-seven individuals of N. uspiana were analysed: 391 males, 163 females, and 293 immatures. Although significant differences in some morphometric parameters were found, there was no sexual dimorphism between males and females. There were differences in total length, width of segments, and length of the notopodial region between matures and immatures. The negative allometry of the total length in relation to five other parameters showed that this feature is a good measure for estimating the individual size, which was then used in the analysis of population structure. This population of N. uspiana showed a bimodal size frequency distribution, with immature and mature individuals found during the entire year. This pattern indicates continuous reproduction, with each cohort growing for at least three to four months and being responsible for two consecutive settlement peaks.

JUVENILE RECRUITMENT, EARLY GROWTH, AND MORPHOLOGICAL VARIATION IN THE ENDANGERED SANTA CATALINA ISLAND RATTLESNAKE, CROTALUS CATALINENSIS

Life-history information constitutes the raw data for building population models used in species conservation. We provide life-history data for the endangered Santa Catalina Island Rattlesnake, Crotalus catalinensis. We use data from 277 observations of C. catalinensis made between 2002 and 2011 on the island. Mean snout-vent length (SVL) of adult C. catalinensis was 643 mm for males and 631 mm for females; the difference was not significant. The degree of sexual size dimorphism (SSD; using SVL) was -0.02. However, sexes were dimorphic in total length ( SVL + tail length), relative tail length, and stoutness. Juvenile recruitment occurs during late-summer. In their first year of life, juveniles seem to grow at a rate of about 1.7 cm/mo. Females seem to become mature around 570 mm SVL, probably in the year when they become 2 y old. Scattered literature data corroborates the time of juvenile recruitment described herein. Growth in C. catalinensis seems to be slower than that of C. ruber, its sister taxa, but similar to other rattlesnakes.

Capillary electrophoretic enantioselective determination of zopiclone and its impurities

A capillary electrophoretic enantioselective method with UV detection was developed and validated for the simultaneous quantification of zopiclone enantiomers and its impurities, zopiclone-N-oxide enantiomers, and 2-amino-5-chloropyridine, in tablets. The analytes were extracted from the tablets using ACN and were separated in an uncoated fused-silica capillary (50 mu m, 42 cm effective length, 50 cm total length) using 80 mM sodium phosphate buffer pH 2.5 and 5 mM carboxymethyl-beta-cyclodextrin as running buffer. The analytes and the internal standard (trimethoprim) were detected at 305 and 200 nm, respectively. A voltage of 27 kV was applied and the capillary temperature was maintained at 25 degrees C. All enantiomers were analyzed within 8 min and linear calibration curves over the concentration range of 0.40.8 mg mL-1 for each zopiclone enantiomer, 0.81.6 mu g mL-1 for 2-amino-5-chloropyridine and 0.40.8 mu g mL-1 for each zopiclone-N-oxide enantiomer were obtained. The coefficients of correlation obtained for the linear curves were greater than 0.99. The intra-day and inter-day accuracy and precision were lower than 2% for all analytes. This validated method was employed to study the degradation and racemization of zopiclone under stress conditions. This application demonstrated the importance of a stability-indicating assay method for this drug.

Morphology and Involution of the Yolk Sac during Early Gestation Bovine (Bos indicus)

Background: The bovine yolk sac derives from visceral endoderm and its development occurs between days 18-23 of gestation. The study of this membrane is important for comparative data and has already been performed in rodents, sheep and in cattle, especially Bos taunts. In species Bos indicus the yolk sac has not quite been studied and is believed that there are morphological differences between these species. The yolk sac undergoes a process of involution and degeneration during embryonic development and none vestige of it is found in late gestation. The period in which occurs the involution of the yolk sac coincides with the period of increased pregnancy loss in cattle, and changes in the morphology of this membrane may indicate the reasons for such high loss rates. Thus, considering that the yolk sac is important for embryonic circulation and metabolic transmission, besides participating actively in the process of cattle placentation, this study aimed characterize morphologically the involution of the bovine yolk sac. Materials, Methods & Results: The early gestational period was determined between days 20 and 70 post-insemination (p.i), according to the exterior characteristics of embryo/fetus. For macroscopic analyzes the uterus was dissected to expose the fetal membranes and subsequently the embryo/fetus was photographed. The samples were fixed for light microscopy and transmission electron microscopy. The yolk sac that emerges from the ventral part of the embryo was prominent and composed by a central part with two thin peripheral projections of different lengths. The bovine yolk sac with about 9 cm on day 25 p. i. of pregnancy permanently decreased its total length during this study. Histologically, the yolk sac is composed of three cell layers: the mesothelium, the mesenchyme and the endoderm. In mesenchyme are found blood islets. In the endoderm are formed cells invaginations toward the mesenchyme originating small canaliculi. The ultrastructure of yolk cells presented many mitochondria, rough endoplasmic reticulum, vesicles, euchromatin and the presence of two nucleoli, Discussion: The real first blood circulation in the bovine is attached with the development of yolk sac, differently from other membranes, such as the corium, that does not present evidence of vascularization by the age of 20-30 days. The erythroblasts found in the yolk sac are related to vasculogenesis and the process of differentiation of blood cells during the erythropoiesis. It could be observed on the histology of the yolk sac, in embryos of 30-50 days old, the presence of canaliculi and small folds of the epithelium. The canaliculi collapse is associated with the degeneration of the endoderm wall of the yolk sac. The organelles present in the endoderm cells of the yolk sac are associated with the function of protein metabolism and in the exchange of substances between the mesenchyme and the mesothelium, For these findings, could be observed that the yolk sac epithelium is found active until the 50th day of gestation, and thereafter regresses. However, remnants of this membrane may be present until the 70th day, These features may represent a presence of an active chorionvitelline placenta in this period responsible for the maintenance of pregnancy whereas the chorioallantoic placenta is not definitively established.

Dynamics of adventitious rooting in mini-cuttings of Eucalyptus benthamii x Eucalyptus dunnii

It is possible to determine the optimum time for permanence of vegetative propagules (mini-cuttings) inside a greenhouse for rooting, and this value can be used to optimize the structure of the nursery. The aim of this study was to determine the dynamics of adventitious rooting in mini-cuttings of three clones of Eucalyptus benthamii x Eucalyptus dunnii. Sprouts of H12, H19 and H20 clones were collected from mini-stumps that were planted in gutters containing sand and grown in a semi-hydroponic system. The basal region of the mini-cuttings was immersed in 2,000 mg L-1 indole-3-butyric acid (IBA) solution for 10 seconds. The rooting percentage of the mini-cuttings, the total length of the root system and the rooting rate per mini-cutting were also evaluated at 0 (time of planting), 7, 14, 21, 28, 35, 42, 49 and 56 days. We used logistic and exponential regression to mathematically model the speed of rhizogenesis. The rooting percentage was best represented as a logistic model, and the total length of the root system was best represented as an exponential model. The clones had different speeds of adventitious rooting. The optimum time for permanence of the mini-cuttings inside the greenhouse for rooting was between 35 and 42 days, and varied depending on the genetic material.